Acetic Anhydride → 1-(2,6-dihydroxyphenyl)-2-methyl-1-propanone O-acetyloxime
反応式
[OH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=[N:13][OH:14])[CH:10]([CH3:12])[CH3:11].[C:15](OC(=O)C)(=[O:17])[CH3:16]>>[C:15]([O:14][N:13]=[C:9]([C:3]1[C:4]([OH:8])=[CH:5][CH:6]=[CH:7][C:2]=1[OH:1])[CH:10]([CH3:12])[CH3:11])(=[O:17])[CH3:16]参加物
3
実験手順
1-(2,6-dihydroxyphenyl)-2-methyl-1-propanone oxime (Intermediate 38, 320 mg) was stirred in acetic anhydride (0.928 ml, 9.84 mmol) at room temperature for 1 hour. After removal of the volatiles, the crude was washed with water, filtered and dried. The residue obtained was charged on a silica gel column (Biotage SP1 system) and eluted with Cyhexane/ethyl acetate (from 100/0 to 0/100) to afford the title compound (127 mg).
後処理
- customAfter removal of the volatiles
- washthe crude was washed with water
- filtrationfiltered
- customdried
- customThe residue obtained
- additionwas charged on a silica gel column (Biotage SP1 system)
- washeluted with Cyhexane/ethyl acetate (from 100/0 to 0/100)
出典と根拠
- ORDレコード
- ord-951341dc2bf7489ab8d50e65c3dc7e09
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09346790B2
反応ノート
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