Stannous Chloride → HCID 57770617、化合物

HRID 1669884ノート

反応式

HRID 1669884 の反応式
[CH3:1][O:2][CH2:3][CH:4]([NH:6][C:7]([C:9]1[CH:10]=[C:11]([C:16]2[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=2)[CH:12]=[C:13]([NH2:15])[CH:14]=1)=[O:8])[CH3:5].[N:23]([O-])=O.[Na+].Cl[Sn]Cl>Cl.O>[CH3:1][O:2][CH2:3][CH:4]([NH:6][C:7]([C:9]1[CH:10]=[C:11]([C:16]2[CH:17]=[CH:18][C:19]([CH3:22])=[CH:20][CH:21]=2)[CH:12]=[C:13]([NH:15][NH2:23])[CH:14]=1)=[O:8])[CH3:5]

参加物

6

反応物 3

HCID 24479Stannous ChlorideHCID 23668193Sodium NitriteHCID 595997035-Amino-4'-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide

生成物 1

HCID 57770617HCID 57770617、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

5-Amino-4′-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide (596 mg, 2 mmol) was dissolved in 6 mL of concentrated HCl and stirred for 15 minutes at 0° C. To the reaction mixture was added a solution of NaNO2 (138 mg, 2 mmol) in water (1.5 mL) dropwise at 0° C. The mixture was stirred for 30 minutes, and then a solution of SnCl2 (4.5 mmol, 189.6 mg) in 2 mL of concentrated HCl was added dropwise. A precipitate began to form immediately. After stirring for another 30 minutes, the resulting 5-hydrazino-4′-methyl-biphenyl-3-carboxylic acid (2-methoxy-1-methyl-ethyl)-amide was isolated as a hydrochloride salt by filtration and immediately used in the next step.

後処理

  1. stirringThe mixture was stirred for 30 minutes
  2. customto form immediately
  3. stirringAfter stirring for another 30 minutes

出典と根拠

ORDレコード
ord-76c4582fdee543b68086e2a392871493
出典データセット
uspto-grants-2011_08
特許番号
US07989637B2

反応ノート

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