Ethanolamine → 2-(4-Chloro-benzylamino)-ethanol

Ethanolamine (56.9 g, 931 mmol) and sodium hydroxide (7.44 g, 186 mmol) were mixed in isopmpanol (50 ml) and 4-chlorobenzyl chloride (30 g, 186 mmol) was added at such a rate that a mild reflux was achieved. The mixture was then refluxed for another 30 min. Evaporation of the solvent was followed by the addition of methylene chloride (50 ml). The solids were filtered off and the solvent was evaporated from the filtrate. The residual oil was distilled under oil pump vacuum and the fraction at 125-126° C. (0.1 mm Hg) was collected. Yield 27 g, 78%.

1. additionwas added at such a rate that
2. temperaturea mild reflux
3. temperatureThe mixture was then refluxed for another 30 min
4. customEvaporation of the solvent
5. additionwas followed by the addition of methylene chloride (50 ml)
6. filtrationThe solids were filtered off
7. customthe solvent was evaporated from the filtrate
8. distillationThe residual oil was distilled under oil pump vacuum
9. customthe fraction at 125-126° C. (0.1 mm Hg) was collected

ORDレコード

ord-d1fe4b5be6be4351a26769edc11cb474

出典データセット

uspto-grants-2002_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06479491B1