常温/回流搅拌
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
反应检测
a. After 1 h, TLC analysis (CH 2 Cl 2 / hexane 3:1) showed the complete consumption ofcompound 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/过夜
a.The mixture was left standing overnight.
b.The mixture was allowed to stand at room temperature for 1 day.
c.The mixture was allowed to stand in a freezer at -15 .℃
4
甲苯/乙醇带水
a.Compound A (1.97 g, 6.63 mmol) was coevaporated with toluene five times to remove the water.
b.The residue was subjected to toluene azeotrope to give the corresponding acid choride as brown oil.
c.The aqueous portion was concentrated under reduced pressure followed by azeotropic removal of water with absolute EtOH.
5
氢化反应
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
The reaction was exothermic / endothermic .
7
微波反应器
The sealed vial was irradiated in the microwave on a Biotage Smith Synthesis at 150℃ for 10 min.
8
反应放热 / 吸热
The reaction was exothermic / endothermic .
9
抽真空
The mixture was degassed for 10 min and refilled with N 2.
10
吸收装置
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
避光反应
a.To the solution which is protected from light was added dropwise Br (3.45 g, 22 mmol) in CH2Cl2 (10 mL) over 5 min and the mixture was stirred for 1 h.
b.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.
