Piperazine → 7-Bromo-6-methoxy-3-(1-piperazinyl)-1,2-benzisoxazole hydrochloride

HRID 582885노트

반응식

HRID 582885 반응식
[Br:1][C:2]1[C:10]2[O:9][N:8]=[C:7]([Cl:11])[C:6]=2[CH:5]=[CH:4][C:3]=1[O:12][CH3:13].[NH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>CO>[ClH:11].[Br:1][C:2]1[C:10]2[O:9][N:8]=[C:7]([N:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[C:6]=2[CH:5]=[CH:4][C:3]=1[O:12][CH3:13]

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 187964507-Bromo-3-chloro-6-methoxy-1,2-benzisoxazole

생성물 1

HCID 187964487-Bromo-6-methoxy-3-(1-piperazinyl)-1,2-benzisoxazole hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
140 °C

실험 절차

To a sealed tube was added 7-bromo-3-chloro-6-methoxy-1,2-benzisoxazole (2.0 g) and piperazine (2.6 g). The reaction was heated to 140° C. over 30 minutes and then cooled to room temperature. The residue was dissolved in MeOH and concentrated in vacuo. Flash column chromatography (silica gel) eluting with 30% MeOH/EtOAc provided a residue upon evaporation (1.0 g) which was recrystallized from MeOH/CH2Cl2 /pet. ether to yield 1.0 g, m.p. 268-269° C.

후처리

  1. temperaturecooled to room temperature
  2. concentrationconcentrated in vacuo
  3. washFlash column chromatography (silica gel) eluting with 30% MeOH/EtOAc
  4. customprovided a residue
  5. customupon evaporation (1.0 g) which
  6. customwas recrystallized from MeOH/CH2Cl2 /pet. ether
  7. customto yield 1.0 g, m.p. 268-269° C.

출처 및 근거

ORD 기록
ord-34c93ea7a5b347b2922fc4709b742496
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925766

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