1-(2-Methoxyphenyl)piperazine → isoquinolin-N-oxide

HRID 638081

반응식

HRID 638081 반응식
COC1C=C(C=CC=1OC)C[C:7]1[C:16]2[C:11](=[CH:12][C:13](OC)=[C:14](OC)[CH:15]=2)[CH:10]=[CH:9][N+:8]=1[O-:21].CN(C)C=O.COC1C=CC=CC=1N1CCNCC1>C(N(CC)CC)C>[CH:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=[CH:9][N+:8]=1[O-:21]

참가 물질

5

반응물 3

HCID 13461-(2-Methoxyphenyl)piperazineHCID 6228DimethylformamideHCID 11810396AGN-PC-00GMS2

생성물 1

HCID 290378isoquinolin-N-oxide

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

A mixture of 2.5g 4-chloromethyl-1-(3,4-dimethoxybenzyl-6,7-dimethoxyisoquinoline 2-oxide, 35 ml dimethylformamide, 1.8 triethylamine and 1.29 g 1-(2-methoxyphenyl)piperazine was stirred and heated under nitrogen at 50° for 7 hours. After evaporation of the solvent, the residue was partitioned between methylene chloride and water. The methylene chloride solution was washed with water and dried. After removal of the solvent in vacuo, the residue (3.5 g) was crystallized from methylene chloride/ethyl acetate to yield 3.05 g of yellow, hygroscopic crystals of 1-(3,4)-dimethoxybenzyl)-6,7-dimethoxy-4-{]4'-(2-methoxyphenyl)-1'-piperazinyl]methyl} isoquinoline 2-oxide, mp 128°-129° (dec.).

후처리

  1. temperatureheated under nitrogen at 50° for 7 hours
  2. customAfter evaporation of the solvent
  3. customthe residue was partitioned between methylene chloride and water
  4. washThe methylene chloride solution was washed with water
  5. customdried
  6. customAfter removal of the solvent in vacuo
  7. customthe residue (3.5 g) was crystallized from methylene chloride/ethyl acetate

출처 및 근거

ORD 기록
ord-a7652a369f1c41c3a08384f1bf64b0d4
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559403

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