Water → HCID 131712977, 화합물

HRID 2296442

반응식

HRID 2296442 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[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.O>CN(C)C=O>[Cl:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[N:5]=[CH:4][N:3]=[C:2]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]

참가 물질

5

반응물 3

HCID 962WaterHCID 6871Diethyl (ethoxymethylene)malonateHCID 3202476-Chloroquinazolin-4-amine

생성물 1

HCID 131712977HCID 131712977, 화합물수율 79.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

A mixture of 4-amino-6-chloroquinazoline (8.7 g) and diethyl ethoxymethylenepropanedioate (11.53 g) in N,N-dimethylformamide (25 ml) was stirred for 2 hours and 40 minutes at 150° C. After the reaction mixture was cooled to ambient temperature, to the mixture was added water with stirring to give crystals, which were washed with water, dried under reduced pressure and dissolved in ethyl acetate under heating. Insoluble materials were filtered off. To the filtrate was added hexane and allowed to stand at ambient temperature to give crystals, which were separated by filtration and washed with a mixture of ethyl acetate and hexane to give a mixture (13.48 g) of crystalline diethyl [(6-chloro-4-quinazolinylamino)methylene]propanedioate and ethyl 10-chloro-4-oxo-4H-pyrimido[1,2-c]quinazoline-3-carboxylate.

후처리

  1. temperatureAfter the reaction mixture was cooled to ambient temperature, to the mixture
  2. stirringwith stirring
  3. customto give crystals, which
  4. washwere washed with water
  5. customdried under reduced pressure
  6. dissolutiondissolved in ethyl acetate
  7. temperatureunder heating
  8. filtrationInsoluble materials were filtered off
  9. additionTo the filtrate was added hexane
  10. customto stand at ambient temperature
  11. customto give crystals, which
  12. customwere separated by filtration
  13. washwashed with a mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-2b8a5ad9b1b545afb88a2b48200c1704
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04429126

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