1-(2-甲氧苯基)哌嗪 → 异喹啉-N-氧化物

HRID 638081

反应方程式

HRID 638081 反应方程式
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]

参与物

5

反应物 3

HCID 13461-(2-甲氧苯基)哌嗪HCID 6228N,N-二甲基甲酰胺HCID 11810396AGN-PC-00GMS2

产物 1

HCID 290378异喹啉-N-氧化物

试剂、催化剂与溶剂 1

HCID 8471三乙胺溶剂

实验过程

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.).

后处理

  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

来源与证据

ORD记录
ord-a7652a369f1c41c3a08384f1bf64b0d4
来源数据集
uspto-grants-1985_12
专利号
US04559403

关联笔记

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