Triethylamine → 2-Bromoethyl methacrylate

An egg-plant type flask which contained benzene (500 ml) was charged with 2-bromoethanol (46.7 g, 0.37 mol) and triethylamine (29.1 g, 0.29 mol) and was capped with a rubber plug. Methacryloyl chloride (30 g, 0.29 mol) was added to the flask in ice water, using a syringe while being stirred with a stirrer. The stirring was continued for some time, and then, the mixture was warmed to a room temperature and was stirred overnight. Triethylamine hydrochloride was removed by suction filtration, and the mixture was washed three times with water (300 ml) to extract the unreacted substance. The mixture was transferred to a conical flask and was dried over anhydrous sodium sulfate. The mixture was concentrated by an evaporator under reduced pressure and purified by vacuum distillation to give a colorless and clear liquid (33.8 g) (yield: 61%).

1. customAn egg-plant type flask which contained
2. customwas capped with a rubber plug
3. stirringwas stirred overnight
4. customTriethylamine hydrochloride was removed by suction filtration
5. washthe mixture was washed three times with water (300 ml)
6. extractionto extract the unreacted substance
7. customThe mixture was transferred to a conical flask
8. dry with materialwas dried over anhydrous sodium sulfate
9. concentrationThe mixture was concentrated by an evaporator under reduced pressure
10. distillationpurified by vacuum distillation

ORD record

ord-74d8c2602791451d9a86dedd8f653ee5

Source dataset

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08394887B2