Potassium periodate → tert-butyl N-(2-oxoethyl)carbamate
反応式
[C:1]([NH:8][CH2:9][CH:10]([OH:13])CO)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].I([O-])(=O)(=O)=O.[K+]>O>[C:1]([NH:8][CH2:9][CH:10]=[O:13])([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]参加物
4
実験手順
3-Bocamino-1,2-propanediol (144.7 g; 0.757 mol) was suspended in water (750 ml) and potassium periodate (191.5 g; 0.833 mol) was added. The mixture was stirred under nitrogen for 2.5 h and the precipitated potassium iodate was removed by filtration and washed once with water (100 ml). The aqueous phase was extracted with chloroform (6×400 ml). The chloroform extracts were dried and evaporated to dryness, in vacuo. Yield 102 g (93%) of an oil. The (bocamino)acetaldehyde was purified by kugelrohr distillation at 84° C. and 0.3 mmHg in two portions. The yield 79 g (77%) of a colorless oil.
後処理
- customthe precipitated potassium iodate was removed by filtration
- washwashed once with water (100 ml)
- extractionThe aqueous phase was extracted with chloroform (6×400 ml)
- dry with materialThe chloroform extracts were dried
- customevaporated to dryness, in vacuo
- distillationThe (bocamino)acetaldehyde was purified by kugelrohr distillation at 84° C.
出典と根拠
- ORDレコード
- ord-be7e821a61eb41e3be15a2c1f4638904
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06713602B1
反応ノート
読み込み中…