Ethyl chloroacetate → HCID 18623221, 화합물

HRID 278899노트

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HRID 278899 반응식
[H-].[Na+].[NH2:3][CH:4]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([F:14])[CH:8]=1)[CH2:5][OH:6].Cl[CH2:16][C:17](OCC)=[O:18]>C1COCC1>[F:14][C:9]1[CH:8]=[C:7]([CH:4]2[NH:3][C:17](=[O:18])[CH2:16][O:6][CH2:5]2)[CH:12]=[CH:11][C:10]=1[F:13]

참가 물질

5

반응물 3

HCID 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 220488782-Amino-2-(3,4-difluorophenyl)ethanol

생성물 1

HCID 18623221HCID 18623221, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

To a suspension of NaH (8.0 mmol, 0.19 g) in 10 mL THF at 0° C. was added a solution of 2-amino-2-(3,4-difluorophenyl)-ethanol (7.51 mmol, 1.3 g) in 20 THF dropwise via an addition funnel and after 30 min ethyl chloroacetate was added dropwise via syringe. The orange colored reaction mixture was stirred for 2 hours at 0° C. and then for 2 hours at 35° C. The solvent was removed and the 5-(3,4-difluoro-phenyl)-morpholin-3-one was isolated as a thick yellow oil (0.5 g). 1H NMR showed that the product was about 85% pure and any attempts to purify it further by column chromatography were not successful. It was used in the next reaction as described below without further purification.

후처리

  1. waitfor 2 hours at 35° C
  2. customThe solvent was removed

출처 및 근거

ORD 기록
ord-d8bb694e3a254c848a822cab6ff9f87c
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362182B1

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