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

HRID 638081

反応式

HRID 638081 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 290378isoquinolin-N-oxide

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-a7652a369f1c41c3a08384f1bf64b0d4
出典データセット
uspto-grants-1985_12
特許番号
US04559403

関連ノート

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