Triethylamine → HCID 57447109、化合物

HRID 2105459ノート

反応式

HRID 2105459 の反応式
[C:1](Cl)(=[O:5])[CH2:2][CH2:3][CH3:4].C(N(CC)CC)C.[NH2:14][C:15]1[CH:16]=[N:17][C:18]2[C:23]([C:24]=1[Cl:25])=[CH:22][CH:21]=[CH:20][CH:19]=2>ClCCl>[Cl:25][C:24]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[N:17]=[CH:16][C:15]=1[NH:14][C:1](=[O:5])[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 8855Butyryl chlorideHCID 8173324-chloroquinolin-3-amine

生成物 1

HCID 57447109HCID 57447109、化合物収率 48.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Butyryl chloride (0.72 mL, 6.94 mmol, 1.2 eq.) and triethylamine (1.13 mL, 8.09 mmol, 1.4 eq) were added to a solution of 3-amino-4-chloroquinoline (1.03 g, 5.78 mmol, 1.0 eq) in anhydrous dichloromethane (25 mL). The reaction mixture was stirred at ambient temperature for 3 hours and then washed sequentially with saturated aqueous sodium bicarbonate and brine, dried over magnesium sulfate, and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel eluting with 3% methanol in dichloromethane) to provide 0.70 g of N-(4-chloroquinolin-3-yl)butyramide.

後処理

  1. washwashed sequentially with saturated aqueous sodium bicarbonate and brine
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product was purified by column chromatography (silica gel eluting with 3% methanol in dichloromethane)

出典と根拠

ORDレコード
ord-8e0bf9398d4840369802837136103411
出典データセット
uspto-grants-2009_08
特許番号
US07579359B2

反応ノート

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