Potassium periodate → tert-butyl N-(2-oxoethyl)carbamate

HRID 50098

反応式

HRID 50098 の反応式
[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

反応物 2

HCID 516896Potassium periodateHCID 4206999tert-butyl N-(2,3-dihydroxypropyl)carbamate

生成物 1

HCID 4247255tert-butyl N-(2-oxoethyl)carbamate

試薬・触媒・溶媒 1

HCID 962Water溶媒

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

  1. customthe precipitated potassium iodate was removed by filtration
  2. washwashed once with water (100 ml)
  3. extractionThe aqueous phase was extracted with chloroform (6×400 ml)
  4. dry with materialThe chloroform extracts were dried
  5. customevaporated to dryness, in vacuo
  6. distillationThe (bocamino)acetaldehyde was purified by kugelrohr distillation at 84° C.

出典と根拠

ORDレコード
ord-f1b1fd289cf747e08cc586886c20c191
出典データセット
uspto-grants-2004_03
特許番号
US06710163B1

関連ノート

読み込み中…