Diethyl (ethoxymethylene)malonate → HCID 86738819, 화합물

HRID 1719936노트

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HRID 1719936 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:12])=[CH:9][CH:10]=2)[N:5]=[CH:4][N:3]=1.C(O[CH:16]=[C:17]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[C:18]([O:20][CH2:21][CH3:22])=[O:19])C>CN(C)C=O>[Cl:12][C:8]1[CH:7]=[C:6]2[C:11]([C:2]([NH:1][CH:16]=[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:23]([O:25][CH2:26][CH3:27])=[O:24])=[N:3][CH:4]=[N:5]2)=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 218256974-AMino-7-chloroquinazoline

생성물 1

HCID 86738819HCID 86738819, 화합물수율 65.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
150 °C

실험 절차

A mixture of 4-amino-7-chloroquinazoline (1.3 g) and diethyl ethoxymethylenepropanedioate (1.72 g) in N,N-dimethylformamide (6 ml) was stirred for 2 hours at 150° C. The resultant mixture was cooled to ambient temperature and poured into ice-water to give crystals, which were separated by filtration, washed with water and recrystallized from ethanol to give a mixture (1.65 g) of diethyl [(7-chloro-4-quinazolinylamino)methylene]propanedioate and ethyl 9-chloro-4-oxo-4H-pyrimido[1,2-c]quinazoline-3-carboxylate. The mixture was subjected to a column chromatography using silica gel (developing solvent: a mixture of benzene and ethyl acetate (10:1)) to give purified crystals.

후처리

  1. customto give crystals, which
  2. customwere separated by filtration
  3. washwashed with water
  4. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-5899e4a1e9184f7e854c4d5e08d518ad
출처 데이터셋
uspto-grants-1985_09
특허 번호
US04543356

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