Triethylamine → HCID 57654660、化合物

HRID 1175167ノート

反応式

HRID 1175167 の反応式
[CH2:1]([O:3][C:4]([C:6]1([CH2:10][NH2:11])[CH2:9][CH2:8][CH2:7]1)=[O:5])[CH3:2].C(N(CC)CC)C.CC(C(Cl)=O)[C:21](Cl)=[O:22].[C:27]([O:30][CH2:31]C)(=[O:29])[CH3:28]>ClCCl>[CH2:1]([O:3][C:4]([C:6]1([CH2:10][NH:11][C:21](=[O:22])[CH2:28][C:27]([O:30][CH3:31])=[O:29])[CH2:9][CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 10931669MethylmalonylchlorideHCID 45122079Ethyl 1-(aminomethyl)cyclobutanecarboxylate

生成物 1

HCID 57654660HCID 57654660、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

1-Aminomethyl-cyclobutanecarboxylic acid ethyl ester (WO2006/100208) (1.26 g, 8.0 mmol) and triethylamine (0.88 ml, 9.6 mmol) are dissolved in 30 ml dichloromethane (DCM). The solution is cooled to 0° C. and methylmalonylchloride (0.88 ml, 8.0 mmol) in 10 ml DCM is added within 15 minutes. The reaction mixture is stirred for 1 hour at 0° C. followed by 72 hours stirring at room temperature. The reaction mixture is diluted with 400 ml ethyl acetate, and washed with NaHCO3 solution, 1N HCl and brine. Evaporation of the solvent provides the title compound as viscous oil. LC-MS (m/z, ES+): 258 (MH+), retention time: 1.28 mins (LC-MS method 8)

後処理

  1. waitfollowed by 72 hours
  2. stirringstirring at room temperature
  3. washwashed with NaHCO3 solution, 1N HCl and brine
  4. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-098985568970476e837d8877df261dee
出典データセット
uspto-grants-2010_11
特許番号
US07838674B2

反応ノート

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