Water → HCID 66836000、化合物

HRID 2404442ノート

反応式

HRID 2404442 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([O:8][CH:9]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([N+:25]([O-])=O)[CH:20]=2)[C:10]2[NH:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[N:11]=2)[CH2:4][CH2:3]1.[Sn+2].O.O.[Cl-].[Cl-].O.[OH-].[Na+]>C(O)C>[NH:11]1[C:12]2[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=2[N:14]=[C:10]1[CH:9]([O:8][CH:5]1[CH2:4][CH2:3][N:2]([CH3:1])[CH2:7][CH2:6]1)[C:19]1[CH:20]=[C:21]([NH2:25])[CH:22]=[CH:23][CH:24]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 10198436Stannous chloride dihydrateHCID 66835904HCID 66835904、化合物

生成物 1

HCID 66836000HCID 66836000、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2-[(1-Methyl-piperidin-4-yloxy)-(3-nitro-phenyl)-methyl]-1H benzimidazole (110 mg) in ethanol (5 mL) is added Tin(II)dichloride-dihydrate (340 mg). The reaction mixture is heated at reflux for 2 hours. Water is added to the mixture as well as sodium hydroxide 1N solution to pH 10 The solution is extracted with chloroform. The pooled organic phases are dried with magnesium sulphate and concentrated under reduced pressure. The residue is purified by chromatography (gradient dichloromethane/methanol/ammonia from 98/2/0.2 to 90/10/1) to give 3-[(1H-benzimidazol-2-yl)(1-methylpiperidin-4-yloxy)methyl]phenylamine that is used without further purification.

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for 2 hours
  3. extractionis extracted with chloroform
  4. dry with materialThe pooled organic phases are dried with magnesium sulphate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is purified by chromatography (gradient dichloromethane/methanol/ammonia from 98/2/0.2 to 90/10/1)

出典と根拠

ORDレコード
ord-17ff6f04536a41a5983946b6c430783b
出典データセット
uspto-grants-2014_08
特許番号
US08802664B2

反応ノート

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