反应方程式
[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[K+].[K+].[OH:12][CH2:13][C:14]1[C:18]2[CH:19]=[C:20]([N:23]3[C:28](=[O:29])[CH:27]=[C:26]([C:30]([F:33])([F:32])[F:31])[N:25]([CH3:34])[C:24]3=[O:35])[CH:21]=[CH:22][C:17]=2[S:16][N:15]=1.CN1C(C(F)(F)F)=CC(=[O:47])N(C2C=CC3SN=C(C=O)C=3C=2)C1=O>S(=O)(=O)(O)O.C(O)(=O)C.O>[CH3:34][N:25]1[C:26]([C:30]([F:32])([F:31])[F:33])=[CH:27][C:28](=[O:29])[N:23]([C:20]2[CH:21]=[CH:22][C:17]3[S:16][N:15]=[C:14]([C:13]([OH:47])=[O:12])[C:18]=3[CH:19]=2)[C:24]1=[O:35]参与物
7
反应物 3
产物 1
试剂、催化剂与溶剂 3
实验过程
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-(hydroxymethyl)-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.).
后处理
- 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
来源与证据
- ORD记录
- ord-565e9ea917874e72a29ac18a98704b66
- 来源数据集
- uspto-grants-2004_03
- 专利号
- US06706663B2
关联笔记
加载中…