Water → HCID 131712977、化合物

HRID 1719935

反応式

HRID 1719935 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 131712977HCID 131712977、化合物収率 79.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-46f470ca4de14052b682120246716b1e
出典データセット
uspto-grants-1985_09
特許番号
US04543356

関連ノート

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