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Water → 8-(2-chloroethylureido)-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran

HRID 1452302
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HRID 1452302 반응식
[Cl:1][CH2:2][CH2:3][N:4]=[C:5]=[O:6].[NH2:7][C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1.O>CN(C)C=O>[Cl:1][CH2:2][CH2:3][NH:4][C:5](=[O:6])[NH:7][C:8]1[C:17]2[O:16][C:15]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)=[C:14]([CH3:24])[C:13](=[O:25])[C:12]=2[CH:11]=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 160352-Chloroethyl isocyanateHCID 199728088-amino-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran

생성물 1

HCID 677147128-(2-chloroethylureido)-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4 ml of 2-chloroethylisocyanate were added, under stirring at ambient temperature, to a solution of 3.9 g of 8-amino-3-methyl-4-oxo-2-phenyl-4H-1-benzopyran in 52 ml of anhydrous dimethylformamide. Stirring was continued at 70° C. for 5 hours. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic phase was evaporated to dryness in vacuo. The residue was suspended in diethyl ether under stirring. The title product was then filtered off and recrystallized from methanol. Yield 3.74 g, m.p. 213°-214° C.

후처리

  1. extractionwas then extracted with ethyl acetate
  2. customThe organic phase was evaporated to dryness in vacuo
  3. stirringunder stirring
  4. filtrationThe title product was then filtered off
  5. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-7083c71f42784ea882f0498213e02909
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05605896

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