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

HRID 1458552노트

반응식

HRID 1458552 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-5349ea0088164e4990ed3ae3e7da87f2
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05852022

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