Water → 3-(6-(4-Cyclopropylpiperazin-1-yl)-pyridazin-3-yl)-phenylamine

HRID 80932ノート

反応式

HRID 80932 の反応式
[CH:1]1([N:4]2[CH2:9][CH2:8][N:7]([C:10]3[N:11]=[N:12][C:13]([C:16]4[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-])=O)[CH:17]=4)=[CH:14][CH:15]=3)[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.O>C(O)C.[Fe]>[CH:1]1([N:4]2[CH2:5][CH2:6][N:7]([C:10]3[N:11]=[N:12][C:13]([C:16]4[CH:17]=[C:18]([NH2:22])[CH:19]=[CH:20][CH:21]=4)=[CH:14][CH:15]=3)[CH2:8][CH2:9]2)[CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 962WaterHCID 580066013-(4-Cyclopropyl-piperazin-1-yl)-6-(3-nitro-phenyl)-pyridazine

生成物 1

HCID 580065533-(6-(4-Cyclopropylpiperazin-1-yl)-pyridazin-3-yl)-phenylamine収率 71.4%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

A solution of 3-(4-cyclopropyl-piperazin-1-yl)-6-(3-nitro-phenyl)-pyridazine (3.60 g, 11 mmol) in ethanol (18 mL) was added to water (30 mL) and powdered Fe (1.86 g, 33 mmol). The mixture was stirred for 3 h at 80° C. The resulting mixture was filtered and the filtrate was extracted with CH2Cl2. The organic phase was washed with brine, dried (Na2SO4) and concentrated to give 2.32 g (71%) of 3-[6-(4-cyclopropyl-piperazin-1-yl)-pyridazin-3-yl]-phenylamine.

後処理

  1. filtrationThe resulting mixture was filtered
  2. extractionthe filtrate was extracted with CH2Cl2
  3. washThe organic phase was washed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6898db00fc1b49ad8fb3b0b36b79c255
出典データセット
uspto-grants-2014_09
特許番号
US08846677B2

反応ノート

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