反应详情

‘880’ Aqueous ammonia solution (5 mL) was added to a solution of 2,2,2-trifluoro-1-(9-(2-fluoro-3-(2-hydroxyethyl)benzyl)-1-oxa-4,9-diazaspiro[5.5]undecan-4-yl)ethanone (example 67, step e) (1.9 g) in methanol (25 mL). The resulting mixture was stirred for 90 min and the solvent evaporated. The residue was purified by silica gel chromatography eluting with 94.5:5:0.5 to 89:10:1 DCM:methanol:‘880’ ammonia gradient. The fractions containing product were combined and evaporated to give a gum that solidified on standing. The white solid was triturated with isohexane and dried over sodium sulphate to give the subtitled compound as a white solid. Yield 1 g.

1. customthe solvent evaporated
2. customThe residue was purified by silica gel chromatography
3. washeluting with 94.5:5:0.5 to 89:10:1 DCM
4. additionThe fractions containing product
5. customevaporated
6. customto give a gum that
7. customThe white solid was triturated with isohexane
8. dry with materialdried over sodium sulphate