Methyl 7-chloro-6-oxoheptanoate → HCID 20202828、化合物

HRID 543781ノート

反応式

HRID 543781 の反応式
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

参加物

4

反応物 2

HCID 15576276Methyl 7-chloro-6-oxoheptanoateHCID 178512206HCID 178512206、化合物

生成物 1

HCID 20202828HCID 20202828、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f4f84448db5c48d2889f6ef096580f2c
出典データセット
uspto-grants-1984_05
特許番号
US04447441

反応ノート

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