Diethyl (ethoxymethylene)malonate → HCID 59255053, 화합물

HRID 1809348노트

반응식

HRID 1809348 반응식
[CH:1]([N:4]=[C:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].C([O:10][CH:11]=[C:12]([C:18](OCC)=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14])C>C1(OC2C=CC=CC=2)C=CC=CC=1>[CH:5]([N:4]1[C:1]([CH3:3])=[CH:2][CH:18]=[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:11]1=[O:10])([CH3:7])[CH3:6]

참가 물질

4

반응물 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 1378922-Propanamine, N-(1-methylethylidene)-

생성물 1

HCID 59255053HCID 59255053, 화합물수율 70%

시약·촉매·용매 1

HCID 7583Diphenyl Ether용매

반응 조건

온도
185 °C

실험 절차

A mixture of isopropyl(1-methylethylidene)amine (7.94 g, 80.0 mmol, prepared according to Newcomb, Martin et al., J. Amer. Chem. Soc., 1990, 112, 5186) and diethyl (ethoxymethylene)malonate (17.31 g, 80.0 mmol) in diphenyl ether (48 mL) was stirred in a sealed tube at 180-190° C. for 18 h. After cooling, the mixture was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1˜1/2) to give 12.5 g (70%) of the title compound as brown oil.

후처리

  1. temperatureAfter cooling
  2. customthe mixture was chromatographed on a column of silica gel eluting with n-hexane/ethyl acetate (v/v=1/1˜1/2)

출처 및 근거

ORD 기록
ord-0148654cfe5b4088a5486aacd9a0647f
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362038B2

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