ethyl N-(2-cyano-3-ethoxyacryloyl)carbamate → 1-(3,3-Diethoxy-propyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidine-5-carbonitrile

HRID 12667

반응식

HRID 12667 반응식
C([O:3][C:4](=O)[NH:5][C:6](=[O:14])[C:7]([C:12]#[N:13])=[CH:8]OCC)C.[CH2:16]([O:18][CH:19]([O:23][CH2:24][CH3:25])[CH2:20][CH2:21][NH2:22])[CH3:17]>O>[CH2:16]([O:18][CH:19]([O:23][CH2:24][CH3:25])[CH2:20][CH2:21][N:22]1[CH:8]=[C:7]([C:12]#[N:13])[C:6](=[O:14])[NH:5][C:4]1=[O:3])[CH3:17]

참가 물질

4

반응물 2

HCID 230015ethyl N-(2-cyano-3-ethoxyacryloyl)carbamateHCID 5210291-Amino-3,3-diethoxypropane

생성물 1

HCID 589941901-(3,3-Diethoxy-propyl)-2,4-dioxo-1,2,3,4-tetrahydro-pyrimidine-5-carbonitrile수율 92.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

(2-Cyano-3-ethoxy-acryloyl)-carbamic acid ethyl ester (Prep 33, 300 mg, 1.42 mmol) was suspended in water (20 mL); 3,3-diethoxypropylamine (460 μl, 2.84 mmol) was added and the mixture warmed at 80° C. for 10 minutes. The reaction mixture was lyophilized and the residue was purified by flash chromatography with petroleum ether-ethyl acetate (1-1) to give 350 mg of the title compound (91% yield)

후처리

  1. customthe residue was purified by flash chromatography with petroleum ether-ethyl acetate (1-1)

출처 및 근거

ORD 기록
ord-62cee4579b5c4dd7a0d29b59c51a8f86
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727988B2

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