Sodium Iodide → HCID 18629502、化合物
反応式
[C:1](=[O:14])([O:5][CH2:6][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[O:2][CH2:3]Cl.[I-:15].[Na+]>C(#N)C>[C:1](=[O:14])([O:5][CH2:6][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[O:2][CH2:3][I:15]参加物
4
反応条件
- 温度
- 40 °C
実験手順
Chloromethyl tert-butoxycarbonylmethyl carbonate (6.45 g) was added to a solution of sodium iodide (16.5 g) in acetonitril (65 ml). After stirring at 40° C. for 4 hours the reaction mixture was cooled in ice, filtered and evaporated in vacuo. The residue was taken up in dichloromethane, washed with aqueous sodium bicarbonate and sodium thiosulfate, dried over magnesium sulfate, filtered and evaporated in vacuo. Purification on silica gel with hexane/ethyl acetate (3:1) as eluent gave the title compound as a colourless oil.
後処理
- temperaturewas cooled in ice
- filtrationfiltered
- customevaporated in vacuo
- washwashed with aqueous sodium bicarbonate and sodium thiosulfate
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo
- customPurification on silica gel with hexane/ethyl acetate (3:1) as eluent
出典と根拠
- ORDレコード
- ord-ff36d2dd32054077ac5a844b06e75a2f
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06525077B2
反応ノート
読み込み中…