HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 22119824, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 5-[3,6-Dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxylic acid | HCID 11187860 | — |
| Catalyst | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 22119824 | HCID 22119824 | 75.3% |
Reaction Steps
To a solution of 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxylic acid (0.300 g, 0.000809 mol) in methanol is added sulfuric acid (98%, 5 drops) at room temperature. The resultant mixture is stirred overnight at room temperature and concentrated in vacuo. The residue is taken up in methylene chloride, washed with saturated sodium bicarbonate and brine, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. Column chromatography of the residue on silica gel with methylene chloride:ethyl acetate gives the title compound as a white solid (0.235 g, 75.3%, mp 153-156° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06156700 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-fd454fdd5838470e894185925c87bf43 |
| Source note | uspto-grants-2000_12 |