반응식
OO.[OH:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([CH2:12][O:13][CH3:14])[N:7]=[C:6](S)[N:5]=1.S(OS([O-])=O)([O-])=O.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+]>>[OH:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([CH2:12][O:13][CH3:14])[N:7]=[CH:6][N:5]=1참가 물질
실험 절차
To 750 ml of 12% strength hydrogen peroxide, heated to 80° C., there were added in portions 101 g (0.5 mol) of 4-hydroxy-2-mercapto-5-methoxy-6-methoxymethylpyrimidine in such a way that a temperature of 80° C. was maintained. Stirring was then continued for 2 hours at 80° C. After cooling, solid sodium disulfite was added until potassium iodide/starch paper no longer showed a reaction with peroxide, and the mixture was then neutralized by adding potassium carbonate. The water was distilled off, and the solid residue, to which a little ethanol had been added, was then suspended in methylene chloride and subjected to filtration with suction. After concentration of the filtrate, 63 g (70% of theory) of product of melting point 141°-143° C. were obtained.
후처리
- temperaturewas maintained
- temperatureAfter cooling
- distillationThe water was distilled off
- additionthe solid residue, to which a little ethanol had been added
- filtrationsubjected to filtration with suction
- customAfter concentration of the filtrate, 63 g (70% of theory) of product of melting point 141°-143° C. were obtained
출처 및 근거
- ORD 기록
- ord-6412ba8167d748be8a527b4d4ed93a35
- 출처 데이터셋
- uspto-grants-1997_09
- 특허 번호
- US05668140
연결된 노트
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