Water → 1-[4-Benzyl-(1-piperazinyl)]isoquinoline

HRID 365293ノート

反応式

HRID 365293 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.[CH2:12]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(CC)C(C)C)(C)C.O>CN(C=O)C>[CH2:12]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]=[CH:4][N:3]=2)[CH2:21][CH2:20]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

6

反応物 4

HCID 962WaterHCID 759941-BenzylpiperazineHCID 81531DiisopropylethylamineHCID 140539Isoquinoline, 1-chloro-

生成物 1

HCID 224680261-[4-Benzyl-(1-piperazinyl)]isoquinoline収率 40.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of 1-chloroisoquinoline (1.64 g 10 mmol) in dry DMF (5 ml) was added to a stirred solution of 1-benzylpiperazine (1.85 g, 10.5 mmol) and N,N-diisopropylethylamine (2 ml, 1.5 g, 11.5 mmol) in dry DMF (5 ml) under Ar at room temperature. The solution was stirred at room temperature for 17 h. The yellow solution was heated at 110° C. for 7 h, treated with water (100 ml) and extracted with ether (2×50 ml). The extracts were dried (Na2SO4) and concentrated in vacuo. The residue was chromatographed (SiO2 ; ethyl acetate) to give the product (1.233 g).

後処理

  1. temperatureThe yellow solution was heated at 110° C. for 7 h
  2. extractionextracted with ether (2×50 ml)
  3. dry with materialThe extracts were dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed (SiO2 ; ethyl acetate)

出典と根拠

ORDレコード
ord-83cf8d208096407f9854c5332bf0ae09
出典データセット
uspto-grants-2000_10
特許番号
US06127357

反応ノート

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