Hexahydro-1,4-diazepine → 3-(1-Homopiperazinyl)-6-methoxy-1,2-benzisoxazole

HRID 1458552ノート

反応式

HRID 1458552 の反応式
Cl[C:2]1[C:6]2[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:5]=2[O:4][N:3]=1.[NH:13]1[CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>CCOC(C)=O>[N:13]1([C:2]2[C:6]3[CH:7]=[CH:8][C:9]([O:11][CH3:12])=[CH:10][C:5]=3[O:4][N:3]=2)[CH2:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1

参加物

4

反応物 2

HCID 68163Hexahydro-1,4-diazepineHCID 158169243-Chloro-6-methoxy-1,2-benzoxazole

生成物 1

HCID 218393333-(1-Homopiperazinyl)-6-methoxy-1,2-benzisoxazole

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
140 °C

実験手順

3-Chloro-6-methoxy-1,2-benzisoxazole (5.0 g, 27.2 mml) and homopiperazine (8.2 g, 81.6 mmol) were combined and mechanically stirred under N2 at 140° C. for 45 minutes. The reaction mixture was cooled to room temperature, dissolved with EtOAc (500 ml), and the solution was washed with water, brine, dried over MgSO4, and concentrated in vacuo. Flash column chromatography (silica gel, 20% MeOH/CH2Cl2) provided the product (2.0 g, m.p. 74°-75° C.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washthe solution was washed with water, brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customFlash column chromatography (silica gel, 20% MeOH/CH2Cl2) provided the product (2.0 g, m.p. 74°-75° C.

出典と根拠

ORDレコード
ord-5349ea0088164e4990ed3ae3e7da87f2
出典データセット
uspto-grants-1998_12
特許番号
US05852022

反応ノート

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