반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([Cl:9])[N:5]=[C:4](C(Cl)(Cl)Cl)[N:3]=1.[OH-:14].[Na+].[ClH:16].[OH2:17]>>[Cl:8][C:7]1[C:6]([OH:17])=[N:5][C:4]([OH:14])=[N:3][C:2]=1[Cl:1].[Cl:16][C:4]1[N:3]=[C:2]([Cl:1])[C:7]([Cl:8])=[C:6]([Cl:9])[N:5]=1참가 물질
실험 절차
242 g of molten 4,5,6-trichloro-2-trichloromethylpyrimidine are metered into a mixture, warmed to 75°-80° C., of 1,200 ml of water, 600 ml of 50% strength sodium hydroxide solution and 15 ml of an emulsifier solution over a heated dropping funnel in the course of 1.5 hours. A rise in temperature to 95° C. is to be observed as a result of exothermic heat of reaction. A clear amber-coloured solution results. After a further hour at 90°-95° C., the reaction solution is cooled and brought to pH 6 with hydrochloric acid. The product which has crystallised out is filtered off with suction, rinsed with about 70 ml of water and dried. 119 g (82% of theory) of a sand-coloured crystalline substance of melting point 302°-303° C. (decomposition) are obtained. The substance proves to be identical, by comparison of the IR and melting point, to 5,6-dichloro-2,4-dihydroxypyrimidine, which was obtained by hydrolysis of 2,4,5,6-tetrachloropyrimidine according to German Offenlegungsschrift 2,153,511. A small amount of 5,6-dichloro-4-hydroxy-2-pyrimidinecarboxylic acid is detectable in the filtrate.
후처리
- customin the course of 1.5 hours
- customto 95° C.
- customa result
- temperatureof exothermic heat of reaction
- customA clear amber-coloured solution results
- waitAfter a further hour at 90°-95° C.
- temperaturethe reaction solution is cooled
- customThe product which has crystallised out
- filtrationis filtered off with suction
- washrinsed with about 70 ml of water
- customdried
- custom119 g (82% of theory) of a sand-coloured crystalline substance of melting point 302°-303° C. (decomposition) are obtained
출처 및 근거
- ORD 기록
- ord-f12c64098d1d4739abaf79df91799801
- 출처 데이터셋
- uspto-grants-1987_04
- 특허 번호
- US04659827
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