HCID 18630005、化合物 → HCID 18630090、化合物
反応式
[CH2:1]([N:3]([CH2:17][O:18]C)[C:4](=[O:16])[C:5]1[C:10]([Si:11]([CH3:14])([CH3:13])[CH3:12])=[CH:9][CH:8]=[CH:7][C:6]=1[CH3:15])[CH3:2]>C(#N)C.Cl>[CH2:1]([N:3]([CH2:17][OH:18])[C:4](=[O:16])[C:5]1[C:10]([Si:11]([CH3:12])([CH3:13])[CH3:14])=[CH:9][CH:8]=[CH:7][C:6]=1[CH3:15])[CH3:2]参加物
4
実験手順
The compound of Example 127 (0.80 g, 2.9 mmol) was refluxed in a mixture of acetonitrile (20 mL) and 2N HCl (20 mL). Within 2 h the reaction was complete by GLC, and was cooled and partitioned between ether and water. The ether phase was concentrated and purified by RC with 1:4 ethyl acetate/hexanes, then recrystallized from hexanes to give 160 mg of the title compound as a solid, a 21% yield.
後処理
- temperaturewas cooled
- custompartitioned between ether and water
- concentrationThe ether phase was concentrated
- custompurified by RC with 1:4 ethyl acetate/hexanes
- customrecrystallized from hexanes
出典と根拠
- ORDレコード
- ord-1363c4345e484970b74522e0c55bda92
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06248894B1
反応ノート
読み込み中…