反应详情

A suspension of 36 g. (0.173 mol) of phosphorous pentachloride in 300 ml. of methylene chloride was treated dropwise with a solution of 37 g. (0.173 mol) of the 2-[[2-(2-chlorophenyl)ethyl]methylamino]ethanol in 150 ml. of methylene chloride. After addition was complete, the mixture was refluxed overnight, evaporated to dryness and partitioned between dilute hydrochloric acid and ether. The aqueous layer was made basic with 10% sodium hydroxide and extracted well with ether. The ether extracts were washed with water and saturated sodium chloride, dried over magnesium sulfate and filtered. Addition of a saturated solution of ethereal hydrochloric acid gave a solid precipitate which was removed by filtration, washed with ether and dried to give 2-chloro-N-(2-chloroethyl)-N-methylbenzene ethanamine hydrochloride, m.p. 110°.

1. additionA suspension of 36 g
2. additionAfter addition
3. temperaturethe mixture was refluxed overnight
4. customevaporated to dryness
5. custompartitioned between dilute hydrochloric acid and ether
6. extractionextracted well with ether
7. washThe ether extracts were washed with water and saturated sodium chloride
8. dry with materialdried over magnesium sulfate
9. filtrationfiltered
10. additionAddition of a saturated solution of ethereal hydrochloric acid
11. customgave a solid precipitate which
12. customwas removed by filtration
13. washwashed with ether
14. customdried