反应详情

Concentrated hydrochloric acid (0.5 mL) was added to a solution of (9-(2-(5-(2-(tert-butyldimethylsilyloxy)ethyl)thiophen-2-yl)ethyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)(2-methylthiazol-4-yl)methanone (example 4, step i) (0.235 g) in methanol (5 mL) and the resulting solution stirred for 1 h. The solvent was evaporated in vacuo and the residue azeotroped with toluene and re-dissolved in methanol (˜2 mL). The residue was dissolved in methanol (10 mL) and applied to a SCX cartridge pre-wetted with methanol. The cartridge was washed with methanol (100 mL) and eluted with 1M ammonia in methanol solution (100 mL). The eluent was evaporated in vacuo to give the subtitled compound as a yellow oil. Yield 0.12 g.

1. customThe solvent was evaporated in vacuo
2. customthe residue azeotroped with toluene
3. dissolutionre-dissolved in methanol (˜2 mL)
4. dissolutionThe residue was dissolved in methanol (10 mL)
5. washThe cartridge was washed with methanol (100 mL)
6. washeluted with 1M ammonia in methanol solution (100 mL)
7. customThe eluent was evaporated in vacuo