反应详情

温度

0 °C

To a suspension of 97% NaH (120 mg, 4.88 mmol) in DMF (10 mL) and DMPU (1 mL) cooled to 0° C., there was added 2-methyl-2-propanethiol (550 mg, 6.10 mmol) and the resulting mixture was stirred at 0° C. for one hour. To this clear solution there was added a solution of product from Step 4 (490 mg, 1.22 mmol) in DMF (4 mL). The mixture was heated at 140° C. for 19 hours, cooled, diluted with H2O, acidified with 1N HCl and extracted 3× with Et2O. These extracts were washed 2× with brine, dried, and evaporated. The residue was chromatographed on silica gel, eluting with a 1:1 mixture of EtOAc and hexane, to afford the title product as a thick oil.

1. temperatureThe mixture was heated at 140° C. for 19 hours
2. temperaturecooled
3. extractionextracted 3× with Et2O
4. washThese extracts were washed 2× with brine
5. customdried
6. customevaporated
7. customThe residue was chromatographed on silica gel
8. washeluting with a 1:1 mixture of EtOAc and hexane