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

HRID 582885ノート

反応式

HRID 582885 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
140 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-34c93ea7a5b347b2922fc4709b742496
出典データセット
uspto-grants-1999_07
特許番号
US05925766

反応ノート

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