2-Methyl-4-(piperazin-1-yl)quinoline → HCID 86691600、化合物

HRID 333972

反応式

HRID 333972 の反応式
[CH3:1][C:2]1[CH:11]=[C:10]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[C:18](Cl)(=[O:23])/[CH:19]=[CH:20]/[CH2:21][CH3:22]>ClCCl>[CH3:1][C:2]1[CH:11]=[C:10]([N:12]2[CH2:17][CH2:16][N:15]([C:18](=[O:23])/[CH:19]=[CH:20]/[CH2:21][CH3:22])[CH2:14][CH2:13]2)[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

参加物

4

反応物 2

HCID 7023182-Methyl-4-(piperazin-1-yl)quinolineHCID 5706546(E)-pent-2-enoyl chloride

生成物 1

HCID 86691600HCID 86691600、化合物収率 88%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

2-Methyl-4-piperazin-1-yl-quinoline (113.7 mg, 0.5 mmol) was dissolved in anhydrous dichloromethane (1 ml), TEA (77 μl, 0.5 mmol) followed by (E)-pent-2-enoyl chloride (65 mg, 0.55 mmol dissolved in 1 ml anhydrous dichloromethane) were added and the mixture was shaken for 15 minutes. The mixture was diluted with dichloromethane, washed with 5% sodium bicarbonate solution and water and the organic phase was evaporated to dryness under reduced pressure. The residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 143 mg of a solid (0.44 mmol, 88%). MS (ES): m/z=354.2 [M+1]+.

後処理

  1. additionwere added
  2. washwashed with 5% sodium bicarbonate solution and water
  3. customthe organic phase was evaporated to dryness under reduced pressure
  4. customThe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)

出典と根拠

ORDレコード
ord-1c2d3493ae7c46c8bd3d6c80eda365e2
出典データセット
uspto-grants-2014_11
特許番号
US08883791B2

関連ノート

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