反应详情

温度

-60 °C

Ethyl(methylsulphanyl)acetate (27.31 mmoles) is added dropwise to a solution of the compound obtained in Step E (23.75 mmoles) in THF (200 ml) at −60° C. under a nitrogen atmosphere. tBuOCl (27.31 mmoles) is added dropwise to the reaction mixture over 20 minutes, keeping the temperature between −60° C. and −55° C. After stirring for 3 hours at −60° C., triethylamine (29.68 mmoles) is added dropwise. The reaction mixture is brought to ambient temperature; aqueous 3M HCl solution (340 ml) is then added and stirring is carried out for a further 2 hours. The organic phase is evaporated and the aqueous suspension is extracted with DCM. The organic phases are combined, then washed with 2M HCl solution and then with saturated NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. The residue is triturated in ethyl ether, filtered and dried in vacuo to yield the title product, which is used directly in the next Step.

1. customthe temperature between −60° C. and −55° C
2. customis brought to ambient temperature
3. stirringstirring
4. waitis carried out for a further 2 hours
5. customThe organic phase is evaporated
6. extractionthe aqueous suspension is extracted with DCM
7. washwashed with 2M HCl solution
8. dry with materialwith saturated NaCl solution, dried over sodium sulphate
9. filtrationfiltered
10. customevaporated to dryness
11. customThe residue is triturated in ethyl ether
12. filtrationfiltered
13. customdried in vacuo