HCID 131731865、化合物 → HCID 67291290、化合物
反応式
[N:1]([CH:4]1[CH2:9][CH2:8][CH2:7][CH:6]([O:10][CH3:11])[CH:5]1[O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14])=[N+]=[N-]>C(OCC)(=O)C.[Pd]>[NH2:1][CH:4]1[CH2:9][CH2:8][CH2:7][CH:6]([O:10][CH3:11])[CH:5]1[O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14]参加物
4
実験手順
A solution of racemic [1-Azido-3-methoxy-2-cyclohexanoxy]tert-butyl-dimethylsilane, 51g, (2.57 g; 6.3 mmol) in 20 mL of ethyl acetate was hydrogenated with Pd—C 10% (5 mole %; Degussa) at 45 PSI in a Parr hydrogenation apparatus for 1 h. The reaction mixture was filtered over a nylon and glass fiber filter and concentrated in vacuo to provide 2.32 g of the desired product 51h as a white solid.
後処理
- filtrationThe reaction mixture was filtered over a nylon and glass fiber
- filtrationfilter
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-5786e7f4d27d4924b1d1d5d541ddd1a1
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08829007B2
反応ノート
読み込み中…