Triethylamine → HCID 57654660, 화합물

HRID 1175167노트

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HRID 1175167 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 57654660HCID 57654660, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

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)

후처리

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

출처 및 근거

ORD 기록
ord-098985568970476e837d8877df261dee
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07838674B2

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