Hydrochloric Acid → N-(3-Chloro-2-hydroxypropyl)acetamide

HRID 1701179노트

반응식

HRID 1701179 반응식
C(Cl)(=[O:3])C.[C:5]1([CH:11]2[NH:15][CH2:14][CH:13]([CH2:16][Cl:17])[O:12]2)C=CC=CC=1.Cl>C(Cl)(Cl)Cl.N1C=CC=CC=1>[C:11]([NH:15][CH2:14][CH:13]([OH:12])[CH2:16][Cl:17])(=[O:3])[CH3:5]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 2707015-(Chloromethyl)-2-phenyl-1,3-oxazolidine

생성물 1

HCID 11286567N-(3-Chloro-2-hydroxypropyl)acetamide수율 65%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6212Chloroform용매

실험 절차

15.7 g of acetylchloride are added dropwise to a solution of 39.5 g of 2-phenyl-5-chloromethyloxazolidine in a mixture of 150 ml of chloroform and 16 ml of pyridine at a temperature of -40° C. under agitation. The solution is allowed to warm up to room temperature. After a reaction period of 14 hours, 100 ml of concentrated hydrochloric acid are added. After thoroughly mixing, the aqueous phase is separated and diluted with water to twice its volume and then is saturated with sodium chloride. By extracting the aqueous phase with methylene chloride, drying the methylene-chloride-extract and evaporating the solvent, 19.7 g of N-acetyl-3-chloro-1-aminopropan-2-ol is obtained as an oil which can be used in the following reaction without any purification.

후처리

  1. additionare added
  2. additionAfter thoroughly mixing
  3. customthe aqueous phase is separated
  4. additiondiluted with water to twice its volume
  5. extractionBy extracting the aqueous phase with methylene chloride
  6. dry with materialdrying the methylene-chloride-
  7. extractionextract
  8. customevaporating the solvent

출처 및 근거

ORD 기록
ord-1bbb07493aa24741b8008d8d84c06484
출처 데이터셋
uspto-grants-1980_03
특허 번호
US04191770

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