Cyclobutylamine → 5-Chloro-N3-cyclobutylpyridazine-3,4-diamine

HRID 1846058ノート

反応式

HRID 1846058 の反応式
Cl[C:2]1[N:3]=[N:4][CH:5]=[C:6]([Cl:9])[C:7]=1[NH2:8].[CH:10]1([NH2:14])[CH2:13][CH2:12][CH2:11]1>O>[Cl:9][C:6]1[C:7]([NH2:8])=[C:2]([NH:14][CH:10]2[CH2:13][CH2:12][CH2:11]2)[N:3]=[N:4][CH:5]=1

参加物

4

反応物 2

HCID 75645CyclobutylamineHCID 64032013,5-Dichloro-1,4-dihydropyridazin-4-imine

生成物 1

HCID 867232805-Chloro-N3-cyclobutylpyridazine-3,4-diamine収率 58%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
125 °C

実験手順

A mixture of 3,5-dichloro-4-aminopyridazine (Preparation 4, 200 mg, 1.22 mmol), cyclobutyl amine (0.56 mL) and water (1.12 mL) was heated under microwave irradiation at 125° C. for 4 hours. The reaction mixture was concentrated in vacuo and the crude residue was purified by silica gel column chromatography eluting with CH2Cl2:MeOH 98:2 to afford the title compound as a brown solid in 58% yield, 140 mg.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe crude residue was purified by silica gel column chromatography
  3. washeluting with CH2Cl2:MeOH 98:2

出典と根拠

ORDレコード
ord-add5d5756e6c4df0b56c1d7bd87cdebc
出典データセット
uspto-grants-2015_02
特許番号
US08952008B2

反応ノート

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