반응식
[Na].[C:2]([C:4]([C:11]#[N:12])=[C:5]([NH:8][C:9]#[N:10])[S:6][CH3:7])#[N:3].[ClH:13]>C(OCC)C>[NH2:10][C:9]1[N:3]=[C:2]([Cl:13])[C:4]([C:11]#[N:12])=[C:5]([S:6][CH3:7])[N:8]=1참가 물질
실험 절차
The compound of formula (56), the sodium salt of 2,2-dicyano-1-methylsulfanyl-vinyl-cyanamide, is reacted by addition to a large excess of anhydrous hydrogen chloride in an ethereal solvent, preferably diethyl ether, at 0° C. and the mixture is allowed to warm slowly to room temperature for over 1-36 hours, preferably 18 hours. The product of formula (57), 2-amino-4-chloro-6-methylsulfanyl-pyrimidine-5-carbonitrile, is isolated by conventional means, and preferably purified by means of recrystallisation or chromatography. Alternatively, the compound of formula (56), the sodium salt of 2,2-dicyano-1-methylsulfanyl-vinyl-cyanamide, is reacted with hydrogen bromide in a protic solvent, preferably acetic acid, at 5° C. and the mixture is allowed to warm slowly to room temperature for over 1-36 hours, preferably 1 hour. The product of formula (57), 2-amino-4-bromo-6-methylsulfanyl-pyrimidine-5-carbonitrile, is isolated by conventional means, and preferably purified by means of recrystallisation or chromatography.
후처리
- customat 0° C.
출처 및 근거
- ORD 기록
- ord-bac4f58810664699a82dab029178f9cc
- 출처 데이터셋
- uspto-grants-2003_07
- 특허 번호
- US06586441B2
연결된 노트
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