Diphenyl disulfide → HCID 12851841, 화합물

HRID 1156899노트

반응식

HRID 1156899 반응식
[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

참가 물질

4

반응물 2

HCID 13436Diphenyl disulfideHCID 12851825HCID 12851825, 화합물

생성물 1

HCID 12851841HCID 12851841, 화합물수율 78.2%

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-94af7538df9847f88417197c86cb9a40
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04337256

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