Trifluoroacetic acid → HCID 178483309、化合物

HRID 220252

反応式

HRID 220252 の反応式
C(O[C:6](=O)[N:7]([CH2:9][CH2:10][C:11]1[NH:15][C:14]2[C:16]([O:20][CH3:21])=[CH:17][CH:18]=[CH:19][C:13]=2[N:12]=1)C)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:21][O:20][C:16]1[C:14]2[NH:15][C:11]([CH2:10][CH2:9][NH:7][CH3:6])=[N:12][C:13]=2[CH:19]=[CH:18][CH:17]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 178488952HCID 178488952、化合物

生成物 1

HCID 178483309HCID 178483309、化合物収率 37.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 1.5 g of [2-(7-methoxy-1H-benzoimidazol-2-yl)-ethyl]-methyl-carbamic acid tert.-butyl ester in 10 mL DCM was treated with 0.39 mL of TFA and stirred overnight at rt. The reaction mixture was concentrated in vacuo, redissolved in DCM and treated with diluted NaOH. After separation of the 2 phases the water phase was lyophilized to yield 380 mg of [2-(7-methoxy-1H-benzoimidazol-2-yl)-ethyl]-methyl-amine as beige solid.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionredissolved in DCM
  3. additiontreated with diluted NaOH
  4. customAfter separation of the 2 phases the water phase

出典と根拠

ORDレコード
ord-9d1d1ccde96d430e95a9e09857093f57
出典データセット
uspto-grants-2012_06
特許番号
US08202885B2

関連ノート

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