반응식
[C:1]([C:3]1[C:4]([NH:15][CH2:16][CH2:17][O:18][CH3:19])=[N:5][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[N:7][CH:8]=1)#[N:2].[CH2:20]([O:22]CC)[CH3:21].C([CH:27]([C:31](Cl)=[O:32])[C:28](Cl)=[O:29])C.O>C(O)C.C(O)(=O)C>[CH2:20]([O:22][C:31]([C:27]1[C:28](=[O:29])[N:15]([CH2:16][CH2:17][O:18][CH3:19])[C:4]2[N:5]=[C:6]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[N:7]=[CH:8][C:3]=2[C:1]=1[NH2:2])=[O:32])[CH3:21]참가 물질
7
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
To 9.3 g. (0.037 mole) of 5-cyano-4-(2-methoxyethylamino)-2-phenyl pyrimidine in 350 ml. of diethyl ether was added 2.8 g. (0.019 mole) of ethyl malonyl chloride and this mixture was stirred at room temperature for 4.5 hours. Then the solid material was filtered off and the filtrate evaporated to dryness. Ethanol was added until a solution was obtained and this solution was added to 0.85 g. (0.057 mole) of Na in ethanol and stirred 20 minutes. A little water was added and the solution was acidified with acetic acid. The solid product was collected on a suction filter and recrystallized from ethanol to give 2.0 g. of product--m.p. 245°-247° C.
후처리
- filtrationThen the solid material was filtered off
- customthe filtrate evaporated to dryness
- additionEthanol was added until a solution
- customwas obtained
- additionthis solution was added to 0.85 g
- customThe solid product was collected on a suction
- filtrationfilter
- customrecrystallized from ethanol
- customto give 2.0 g
출처 및 근거
- ORD 기록
- ord-6615560cc7d140288f49715af4d0ef1c
- 출처 데이터셋
- uspto-grants-1981_11
- 특허 번호
- US04301281
연결된 노트
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