訂購/客服熱線:137-9521-9287
當前位置:首頁 ? 珂臻學苑

實驗記錄常用英文表達句型

發布時間:2016-10-23

一、 加料過程常用表述
1. 添加試劑
2. 催化量的
3. 氣體保護
4. 通入氣體
5. 通過雙針頭導管加料
6. 通過注射器加料
二、 反應過程常用表述
1. 反應檢測
2. 放置過液
3. 甲苯/乙醇帶水
4. 氫化反應
5. 分水器
6. 反應放熱
7. 微波反應
三、 后處理過程常用表述
1. 過濾
2. 淬火
3. 磨碎
4. 在兩相中分開
5. 靜止固化
6. 在凍干機凍干
7. 純化
過柱
制備 HPLC 純化
制備 TLC 純化
重結晶
8. 調 PH
9. 萃取
10. 濃縮
11. 干燥
干燥
真空干燥
四、 部分常見反應現象描述
1. 加料放熱
2. 反應過程中或者降溫有固體析出
3. 加料不溶解
4. 反應變粘稠/變色
五、 特殊結果敘述
1. 無進一步處理
2. 統一和其他批次一起后處理
3. 檢測條件,不需要后處理
1
一、加料過程常用表述
1.添加試劑
To a mixture (suspension / solution / slurry) of compound 12 (487 mg, 1 mmol) and
o-plenylenediamine (948 mg, 6 mmol) in CH 2 Cl 2 (15 ml) being coolen to 0℃ was
added the DCC (226 mg, 1.1 mmol).
Anhydrous lithium iodide (1.38 g, 10.3 mmol) was added the five portions (dropwise /
in one portion / in portions) to a stirred solution of compound 12 (10.90 g, 51.5 mmol)
in CH 2 Cl 2 (120 ml).
A round-bottom flask was changed with compound 3 (1.75 g, 5.27 mmol), LiCl (1.17
g, 26.3 mmol), DMSO (100 Ml) and H 2 O (378 ul)
分批加入 in portions/portionwise
一次性加入 in one portion
滴加 dropwise
2.催化量的
Et 3 N (20 mL, 142 mmol) and a catalytic amount of DMAP were added the solution of
compound 1 (4.549 g, 46.4 mmol) in CH 2 Cl 2 (120 ml) at 0℃
3.氣體保護
To a stirred -78 solution ℃ of trimethylsilyacetylene (4.44g, 45.5 mmol)in THF (10 ml)
under argon was added dropwise n-butylithium (1.6M in hexane, 28.25 ml).
4.通入氣體
An ozone-enrichen steam of oxygen was bubbled through a cold (-78 ) solution of ℃
compound 9 (128 mg, 1.409 mmol) in CH 2 Cl 2 (5 ml) until it turned light blue. The
solution was purged with argon at -78 for 10 min to remove the excess O ℃
3 .
5.通過雙針頭導管加料
The mixture was added to a sulotion of compound 2 (3.00 g, 12.8 mmol) in THF (48
ml) via cannula over a period of 30 min.
A solution of compound 29 (100 mg, 0.19 mmol, 1.0 equiv) in dry DMSO (1.5 ml)
was cannulated under argon to a vigorously stirred mixture of powered potassium
superoxide (62 mg, 0.87 mmol, 4.5 equiv) and 18-crown-6-ether (23 mg, 0.087 mmol,
0.45 equiv) in dry DMSO (0.5 ml).
2
6.通過注射器加料
To a stirred solution of compound 15 (8.61 g, 21.2 mmol) was added a solution of
p-toluenesulfonic acid (6.0 g) in CH 2 Cl 2 via syringe over 5 min.
7. 反應控溫
A solution of compound 1 (10 g, 1 mol) in EtOAc (20 ml) was added dropwise (via
addition funnel or syringe) to the above mixture at 10 ℃
(while maintaining gentle reflux;
while keeping internal temperature between 10 ℃ – 30 ) ℃ .
二、反應過程常用表述
1. 常溫/回流攪拌
a. The reaction mixture (solution or suspension) was stirred at 5 for 2 hrs and ℃
then kept at room temperature (or ambient temperature) for another 2 hrs (or
overnight)
b. The reaction mixture (solution or suspension) was refluxed (or heated to reflux)
for 2 hrs (or overnight)
c. The reaction mixture (solution or suspension) was heated at 60 for 2 hrs (or ℃
overnight)
d. The reaction mixture (solution or suspension) was allowed to reflux (or heat to
reflux) for 2 hrs (or overnight)
2. 反應檢測
a. After 1 h, TLC analysis (CH 2 Cl 2 / hexane 3:1) showed the complete consumption of
compound 15.
b. The reaction was complete (incomplete or messy) detected by TLC (Petroleum
ether/EtOAc = 4:1),LC-MS, HPLC or NMR.
3. 放置/過夜
The mixture was left standing overnight.
The mixture was allowed to stand at room temperature for 1 day.
The mixture was allowed to stand in a freezer at -15 . ℃
3
4. 甲苯/乙醇帶水
Compound A (1.97 g, 6.63 mmol) was coevaporated with toluene five times to
remove the water. The residue was subjected to toluene azeotrope to give the
corresponding acid choride as brown oil. The aqueous portion was concentrated under
reduced pressure followed by azeotropic removal of water with absolute EtOH.
5. 氫化反應
A mixture of compound 1 (190 g, 0.88 mmol) and Raney Ni (20 g) in ethanol (1500
ml) and ethyl acetate (500 ml) was stirred under 1 atm at room temperature for an
hour.
6. 分水器
A mixture of TsOH.H 2 O (56.91 g. 0.3 mol) and toluene (400 mL) was heated to reflux
to remove water by Dean-Stark trap.
7. 反應放熱 / 吸熱
The reaction was exothermic / endothermic .
8. 微波反應
The sealed vial was irradiated in the microwave on a Biotage Smith Synthesis at
150 for 10 min. ℃
9. 抽真空
The mixture was degassed for 10 min and refilled with N .
2
10. 吸收裝置
The device for absorbing the evolved hydrogen bromide was attched to the reaction
flask. [care!! The reaction evolves HBr and is best connected to a HBr gas trap
(bubber containing 1 M NaOH solution)].
11.避光反應
To the solution which is protected from light was added dropwise Br (3.45 g, 22
mmol) in CH
2
2 Cl 2 (10 mL) over 5 min and the mixture was stirred for 1 h.
A mixture of compound 8 (213 mg, 0.186 mmol) and compound 9 (220 mg, 0.279
mmol) was refluxed for 20h under dark in a nitrogen atmsophere.
4
三、后處理過程常用表述
1. 過濾
The mixture was filtered through a Celite pad, and the filtrate was concentrated to
give the crude product.
2. 淬火
The reaction mixture was quenched by the addition of the saturated aqueous NH 4 Cl.
3. 磨碎
The residue was triturated with ether and filtered to afford a white solid.
4. 分液
After quenching the reaction, the reaction mixture was poured into separator funnel
and separated.
5. 在兩相中分開
The residue was partitioned between ethyl acetate (100 ml) and HCl (1N, 50 ml).The
organic layer was washed with water, dried (MgSO 4 ) and evaporated to dryness.
Ethyl acetate (100 ml) and HCl(1 M aq, 50 mL) were added to the residue, and the
layers were separated.
6. 靜止固化
The crude product was purified by prep-HPLC to give compound 4 as colorless thick
oil, which was solidfied on standing.
7. 在凍干機凍干
The white solid was re-crystallized from water, dried by hyophilization to give a
white solid.
7.純化
7.1 過柱
The crude produt was chromatographed on silica gel (CH 2 Cl 2 / MeOH
20:1→10:1→5:1) to give the compond 8 (0.282 g, 51%) as a white solid.
5
The crude product was purified by column chromatography on silica gel eluted with
(CH 2 Cl 2 / MeOH 20:1→10:1→5:1) to give the compound 8 (0.282 g, 51%) as a white
solid.
7.2 制備 HPLC 純化
Be purified by prep-HPLC to afford/give/yield
7.3 制備 TLC 純化
Be purified by prepare TLC to afford/give/yield
7.4 重結晶
Recrystallized from
8.調 PH
The pH was adjusted to around 9 by progressively adding solid NaHCO 3 .
The mixture was adjusted to pH 9 with solid NaHCO 3 .
酸化: be acidified to 堿化: be basified to 中和: be neutralized
9.萃取
The aqueous layer was extracted with ethyl acetate (100 mL×4).
10.濃縮
The mixture was evaporated to afford the crude product.
The mixture was concentrated afford the crude product.
The solvent was removed to afford the crude product.
11.干燥
11.1 常規干燥
The organic layer was dried over , and concentrated.
4
MgSO
11.2 真空干燥
The precipitate was filtered and dried (in/under vacumm; under reduced pressure).
6
四、部分常見反應現象表述
1.加料加熱
A gentle reflux appeared throughout the addition.
The temperature was increased from 25 ℃ to 50 during the addition. ℃
2.反應過程中或者降溫有固體析出
Solid was precipitate out after 1h reaction.
The reaction mixture was cooled to -10 , and solid was precipitate out. ℃
3.加料不溶解
XX was added to the mixture, and the resulting suspension was stirred for 2h.
4.加熱溶解
The suspension was heated to 90 and stirred until all solid was dissolved. ℃
5.反應變粘稠/變色
The reaction mixture became sticky after 2hrs reaction/stirring.
After 2hrs stirring, the mixture turned into black/brown/gray/yellow/red color.
五、特殊結果敘述
1. 無進一步處理
No further operation
2. 統一和其他批次一起后處理
The work-up of this batch was together with the other batches that recorded in the
following pages.
3. 檢測條件,不需要后處理
IPC check showed this condition is better/bad for this reaction. No further operation /
screen reaction.
7
Processs 組關于實驗記錄本內容方面的規范
1. 反應時間要明確,統一規定為:
XX(時): XX(分) 投料
XX(時): XX(分) 檢測
XX(時): XX(分) 后處理
XX(時): XX(分) 純化及結果
2. 反應必須有重要的反應現象敘述,包括物理現象和化學現象,比如放熱,產
生氣體,產生沉淀,變粘稠,顏色變化等等。
3. 加料過程必須詳細,如加料時的溫度,及加料過程中的溫度變化等,是否滴
加(dropwise), 快速加(quickly),還是分批加(in portions);滴加的話,寫清
楚大概的滴加時間。
4. 反應必須有應有的檢測,并必須寫明是用什么檢測(TLC,HPLC,LC-MS 等)
TLC 的話,要在右下角劃上 TLC 圖,圖上應如實反應你的點板情況,一般包含
3 個點,反應原料點,反應液點和二者的混合點;同時,TLC 還請標明展開劑及
配比
HPLC 或 LC-MC 等檢測請簡要描述檢測結果,如反應基本完全,或者原料和產
物比例 X%: X%等等。
5. 反應后處理必須有詳細敘述(摸索條件不做后處理的例外),包括用什么萃取,
萃取量,萃取次數(以上均可以為概數),后處理中調整酸堿度的需注明用什么
試劑,試劑的狀態(飽和的,X%濃度的等等),調整后的 pH 值,調整過程中需
要注意事項(如,是否滴加調到 pH 9,是否攪拌情況下調整 pH 值,等等)
6. 反應的純化過程必須詳細(無純化的除外),必須寫明。
7. 反應必須有反應結果和反應目的。一個失敗的反應必須闡明原因,摸索條件
的反應必須寫明改反應是測試條件,不需要后處理或者純化,而且,必須寫明通
過檢測條件是否可行,或者同時開展的幾個摸索條件的反應可以橫向進行比較,
哪個條件為最優等,一個完整的反應結果包括理論產量,實際產量,產率,相關
標準品譜圖信息(核磁直接用核磁譜圖的完整標題記錄譜圖信息,HPLC 或者
MC 需要在前面標明是 HPLC 還是 MS),實驗記錄者簽名,實驗記錄結束日期。
8
Notebook 記錄注意事項:
1. 記錄一定要準確,詳實。不要漏記任何信息。比如:展開劑,洗脫液及其比
例;后處理;重結晶試劑的量等。做到能夠被重復。
2. 對于 Sourse; M. W; W.T; Mole (eq.)必須寫全,如果某試劑有危險需要戴
防毒面具等,需要在 Note 中寫明。對于 Source, 如果是中間體,寫出它的 batch
NO;如果是原料,國產的,寫 domestic;如果是進口試劑,寫出公司名稱和試劑
ID 號,如 Aidrich 163767
3. 譜圖編號要寫出。在記錄的時候,在過程中如果打譜了,不論結果如何,都
要寫出編號,且用括號括起來。公司的記錄本則在相應的位置寫出。
4. TLC 版的圖示可在各頁右側標出。最好用尺子畫,便于整條美觀。公司的記
錄本則在相應的位置寫出。
5. 一個實驗完成后,在接下來的記錄頁上的空白處畫一斜線(/)。
6. 如果一個實驗今天沒做完,在記錄的右側寫上日期和姓名,在下一行畫一橫
線,第二天接著做后處理等再記錄的時候,在左邊寫上日期(見實例所示)。
7. 記錄本應每天拿給組長或指定人員審閱一次。
8. 記錄本必須當天記錄。
9. 如果一個實驗沒有在接下來的一頁上書寫,而在其他頁上繼續寫的時候,在
此頁寫末尾寫上“Continued to page”。
10. 所有的反應均應有相關記錄不論反應成功與否。反應數的統計以實驗記錄為
準。
11. 對于一些非標準的縮寫,可以一直寫全稱,也可以在第一次寫的時候在括號
內注明全稱,然后在目錄頁中專門來標明這些縮寫。鑒于很多同事反映目錄頁不
夠用,所以建議寫全稱。
12. 對于一個能被解釋的反應寫明失敗,描述必須事實地,客觀地,并且有數據
支持的,如果不再繼續此反應,必須說明原因;如果某反應不能達到預期的結果,
必須客觀地描述結果。
9