Diphenyl disulfide → HCID 12851841、化合物

HRID 1156899ノート

反応式

HRID 1156899 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[C:13]([Cl:18])[CH:14]=[CH:15][CH:16]=3)[CH2:11][CH2:10][N:9]=2)=[CH:4][CH:3]=1.C1(SSC2C=CC=CC=2)C=CC=CC=1>C1CCCCC1>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:17]3[C:12](=[C:13]([Cl:18])[CH:14]=[CH:15][CH:16]=3)[CH:11]=[CH:10][N:9]=2)=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 13436Diphenyl disulfideHCID 12851825HCID 12851825、化合物

生成物 1

HCID 12851841HCID 12851841、化合物収率 78.2%

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

実験手順

1-(4-Methylphenyl)-5-chloro-3,4-dihydroisoquinoline (29 g) and 24.7 g of diphenyl disulfide were reacted over an oil bath at 220° C. The reaction mixture was dissolved in cyclohexane, and extracted with a 4 N aqueous solution of hydrochloric acid. The aqueous layer was neutralized with an aqueous solution of sodium hydroxide. The resulting oily product was extracted with benzene, washed in water, and dried. The solvent was distilled off, and the residue was recrystallized from benzene to afford 22.5 g of 1-(4-methylphenyl)-5-chloroisoquinoline as colorless needles having a melting point of 88.6° to 89.1° C.

後処理

  1. extractionextracted with a 4 N aqueous solution of hydrochloric acid
  2. extractionThe resulting oily product was extracted with benzene
  3. washwashed in water
  4. customdried
  5. distillationThe solvent was distilled off
  6. customthe residue was recrystallized from benzene

出典と根拠

ORDレコード
ord-94af7538df9847f88417197c86cb9a40
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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