反应详情

温度

0 °C

Methanesulfonyl chloride (44.8 g, 0.4 mol) was added dropwise to a cooled and stirred solution of compound of example 2 (100 g, 0.35 mol) and triethylamine (71.88 g, 0.7 mol) in dry THF (1.0 L). The reaction mixture was further stirred for 45 min. at 0° C. The precipitate of triethylamine HCl was filtered and washed with dry THF (2×100 mL). The filtrate was added dropwise to a refluxing suspension of sodium acetate (115 g, 1.42 mol) in 2-propanol (1.0 L). The reaction mixture was refluxed for a further 15 min., diluted with EtOAc (1.0 L) and salts were filtered. The mixture of salts was washed with EtOAc (2×100 mL). The combined filtrate was concentrated to give a gum. Water (50 mL) was added to the gum with stirring to obtain a solid which was filtered and dried to yield the title compound.

1. temperaturea cooled
2. filtrationThe precipitate of triethylamine HCl was filtered
3. washwashed with dry THF (2×100 mL)
4. temperatureThe reaction mixture was refluxed for a further 15 min.
5. filtrationwere filtered
6. additionThe mixture of salts
7. washwas washed with EtOAc (2×100 mL)
8. concentrationThe combined filtrate was concentrated
9. customto give a gum
10. stirringwith stirring
11. customto obtain a solid which
12. filtrationwas filtered
13. customdried