Chlorosulfonic acid → HCID 14653249、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[CH:16][S:17][C:11]=2[N:10]=[C:9]1[CH3:18].[Cl:19][S:20](O)(=[O:22])=[O:21]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:13](=[O:14])[C:12]2[CH:15]=[C:16]([S:20]([Cl:19])(=[O:22])=[O:21])[S:17][C:11]=2[N:10]=[C:9]1[CH3:18]参加物
3
実験手順
To 140 ml of chlorosulfonic acid was added little by little 54.8 g of 3,4-dihydro-3-(2-chlorophenyl)-2-methyl-4-oxothieno[2,3-d]pyrimidine. After the mixture was heated at 70°-75° C. on the oil bath and stirred for 1.5 hours, the reaction mixture was cooled and then poured onto 2 l of icewater carefully. The precipitated crystals were collected by suction-filtration to afford 65 g of the title compound, m.p. 172°-174° C.
後処理
- temperatureAfter the mixture was heated at 70°-75° C. on the oil bath
- temperaturethe reaction mixture was cooled
- additionpoured onto 2 l of icewater carefully
- filtrationThe precipitated crystals were collected by suction-filtration