Tert-Butylamine → 4-(tert-Butylamino)-4-oxobutanoic acid

HRID 2061233ノート

反応式

HRID 2061233 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH2:3][CH2:2]1.[C:8]([NH2:12])([CH3:11])([CH3:10])[CH3:9]>ClCCl>[C:8]([NH:12][C:1](=[O:7])[CH2:2][CH2:3][C:4]([OH:6])=[O:5])([CH3:11])([CH3:10])[CH3:9]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 7922Succinic anhydride

生成物 1

HCID 2450094-(tert-Butylamino)-4-oxobutanoic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3.07 g (30.6 mmol) of succinic anhydride was suspended in 30 ml of dichloromethane. 4.1 ml (34.5 mmol) of t-butylamine was dropped into the suspension, and the resultant mixture was stirred at room temperature for 1 hour. White crystals thus formed were washed with ethyl acetate and then dissolved in 40 ml of 1 N aqueous sodium hydroxide solution. The resultant solution was stirred at room temperature for 2 hours and then acidified with 1 N aqueous hydrochloric acid solution under cooling with ice. After extracting with ethyl acetate, the organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure to obtain the title compound.

後処理

  1. customWhite crystals thus formed
  2. washwere washed with ethyl acetate
  3. dissolutiondissolved in 40 ml of 1 N aqueous sodium hydroxide solution
  4. temperatureunder cooling with ice
  5. extractionAfter extracting with ethyl acetate
  6. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-c366d52184104f10ba2610b45b3f6d91
出典データセット
uspto-grants-2012_10
特許番号
US08278329B2

反応ノート

読み込み中…