Water → HCID 12851833、化合物

HRID 1156871ノート

反応式

HRID 1156871 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[C:13]([CH2:18]O)[CH:14]=[CH:15][CH:16]=3)[CH:11]=[CH:10][N:9]=2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:22])=O.O.[OH-].[Na+]>O1CCCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[C:13]([CH2:18][Cl:22])[CH:14]=[CH:15][CH:16]=3)[CH:11]=[CH:10][N:9]=2)=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 128518321-(4-Bromophenyl)-5-hydroxymethylisoquinoline

生成物 1

HCID 12851833HCID 12851833、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-(4-Bromophenyl)-5-hydroxymethylisoquinoline (17 g) was dissolved in 300 ml of tetrahydrofuran, and 15 ml of phosphorus oxychloride was added. The mixture was stirred at room temperature for 1 hour. After the reaction, water was added, and the reaction mixture was neutralized with an aqueous solution of sodium hydroxide. The mixture was extracted with benzene, and dried. The solvent was distilled off. The residue was recrystallized from ether-hexane to afford 13.2 g of 1-(4-bromophenyl)-5-chloromethylisoquinoline as colorless prisms having a melting point of 115.5° to 118.5° C.

後処理

  1. additionwas added
  2. extractionThe mixture was extracted with benzene
  3. customdried
  4. distillationThe solvent was distilled off
  5. customThe residue was recrystallized from ether-hexane

出典と根拠

ORDレコード
ord-c9da68286df54d1c92ed69eaca25b59c
出典データセット
uspto-grants-1982_06
特許番号
US04337256

反応ノート

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