반응식
[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=[O:2].[K+].[K+].[CH3:12][N:13]1[C:18]([C:19]([F:22])([F:21])[F:20])=[CH:17][C:16](=[O:23])[N:15]([C:24]2[CH:25]=[CH:26][C:27]3[S:31][N:30]=[C:29]([CH:32]=[O:33])[C:28]=3[CH:34]=2)[C:14]1=[O:35]>S(=O)(=O)(O)O.C(O)(=O)C.O>[CH3:12][N:13]1[C:18]([C:19]([F:20])([F:21])[F:22])=[CH:17][C:16](=[O:23])[N:15]([C:24]2[CH:25]=[CH:26][C:27]3[S:31][N:30]=[C:29]([C:32]([OH:2])=[O:33])[C:28]=3[CH:34]=2)[C:14]1=[O:35]참가 물질
6
반응물 2
생성물 1
시약·촉매·용매 3
실험 절차
A solution of potassium dichromate (10.0 g) in 1.5 M sulfuric acid (200 mL) is cooled to 0° C., treated dropwise with a solution of a 2:3 mixture of 3-[3-(hydromethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione and 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxaldehyde (12.0 g) in acetic acid, stirred at room temperature for 2 hours, and diluted with water. The resultant aqueous mixture is extracted with methylene chloride. The organic extracts are combined, washed sequentially with water and brine, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as a white solid (8.50 g, mp 149-152° C.).
후처리
- extractionThe resultant aqueous mixture is extracted with methylene chloride
- washwashed sequentially with water and brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-50cae551cddb4cf8ac54d8ea1354bcf1
- 출처 데이터셋
- uspto-grants-2000_12
- 특허 번호
- US06156700
연결된 노트
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