Methyl 7-chloro-6-oxoheptanoate → HCID 20202828, 화합물

HRID 543781노트

반응식

HRID 543781 반응식
Cl[CH2:2][C:3](=O)[CH2:4][CH2:5][CH2:6][CH2:7][C:8]([O:10][CH3:11])=[O:9].[F:13][C:14]([F:24])([F:23])[CH2:15][NH:16][C:17]([NH:19][C:20]([NH2:22])=[S:21])=[NH:18]>CCO>[F:24][C:14]([F:13])([F:23])[CH2:15][N:16]=[C:17]([NH2:18])[NH:19][C:20]1[S:21][CH:2]=[C:3]([CH2:4][CH2:5][CH2:6][CH2:7][C:8]([O:10][CH3:11])=[O:9])[N:22]=1

참가 물질

4

반응물 2

HCID 15576276Methyl 7-chloro-6-oxoheptanoateHCID 178512206HCID 178512206, 화합물

생성물 1

HCID 20202828HCID 20202828, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a solution of methyl 7-chloro-6-oxoheptanoate (2.0 g.) in hot EtOH (20 ml.) was added a solution of 2,2,2-trifluoroethylamidinothiourea (2.1 g.) in hot EtOH (20 ml.). The resulting mixture was heated under reflux for 1 hour. The mixture was then evaporated to dryness and the residue partitioned between ether (20 ml.) and water (60 ml.). The aqueous layer was separated and basified with sodium bicarbonate and extracted with EtOAc. The EtOAc solution was evaporated to dryness and the residue crystallised from EtOAc/ether containing a small amount of acetone to give methyl 5-[2-(2-[2,2,2-trifluoroethyl]guanidino)thiazol-4-yl]valerate which was used without further purification.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 1 hour
  3. customThe mixture was then evaporated to dryness
  4. customthe residue partitioned between ether (20 ml.) and water (60 ml.)
  5. customThe aqueous layer was separated
  6. extractionextracted with EtOAc
  7. customThe EtOAc solution was evaporated to dryness
  8. customthe residue crystallised from EtOAc/ether containing a small amount of acetone

출처 및 근거

ORD 기록
ord-f4f84448db5c48d2889f6ef096580f2c
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04447441

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