Dichloromethane → Clopidogrel

HRID 1673061ノート

反応式

HRID 1673061 の反応式
[CH3:1][O:2][C:3]([C@@H:5]([N:13]1[CH2:18][C:17]2[CH:19]=[CH:20][S:21][C:16]=2[CH2:15][CH2:14]1)[C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:4].Cl.C(Cl)Cl.C(=O)([O-])[O-].[K+].[K+]>O>[CH3:1][O:2][C:3]([C@@H:5]([N:13]1[CH2:18][C:17]2[CH:19]=[CH:20][S:21][C:16]=2[CH2:15][CH2:14]1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=1[Cl:12])=[O:4]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 9798860Clopidogrel Hydrochloride

生成物 1

HCID 60606Clopidogrel

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Under the protection of nitrogen gas, clopidogrel hydrochloride (7.15 g) was introduced into methylene dichloride (100 ml) in a 250 ml flask under stirring and cooling with ice water. Then a solution of potassium carbonate (2.5 g) in de-ionized water (30 ml) was added drop by drop into the flask and it was stirred for one hour. The pH value of the upper aqueous phase was kept over 9. The lower organic phase was separated and the aqueous phase was extracted with methylene dichloride (50 ml). The organic phases were combined and dried over sodium sulfate and then concentrated to obtain a free clopidogrel base.

後処理

  1. stirringwas stirred for one hour
  2. customThe lower organic phase was separated
  3. extractionthe aqueous phase was extracted with methylene dichloride (50 ml)
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-da6f826fad2546f5a6addd043d44c31c
出典データセット
uspto-grants-2011_08
特許番号
US07999106B2

反応ノート

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