Sulfuric Acid → N-tert-Butyl-3,3-dimethyl-2-oxobutanamide

HRID 67198

反応式

HRID 67198 の反応式
[C:1]([C:7]#[N:8])(=[O:6])[C:2]([CH3:5])([CH3:4])[CH3:3].CO[C:11]([CH3:14])([CH3:13])[CH3:12].S(=O)(=O)(O)[OH:16]>C(O)(=O)C>[C:11]([NH:8][C:7](=[O:16])[C:1]([C:2]([CH3:5])([CH3:4])[CH3:3])=[O:6])([CH3:14])([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 15413tert-Butyl methyl etherHCID 945273,3-Dimethyl-2-oxobutanenitrile

生成物 1

HCID 13355144N-tert-Butyl-3,3-dimethyl-2-oxobutanamide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

27.8 (0.25 mole) of pivaloyl cyanide, dissolved in 22 g (0.25 mole) of t-butyl methyl ether were added to a reaction mixture, which had been initially introduced into the reaction vessel, consisting of 37.5 g of concentrated sulphuric acid and 52.5 g of glacial acetic acid at 20° to 30° C. in the course of 30 minutes. After subsequently stirring the reaction mixture at room temperature for 2 hours, it was poured onto 125 g of ice and stirred thoroughly. The product which precipitated was filtered off, washed with water and dried. 40.8 g (87.5% of theory) of analytically pure trimethylpyruvic acid N-tert.-butylamide with a melting point of 65° C. and a content of >99% (determined by gas chromatography) were obtained.

後処理

  1. additionwere added to a reaction mixture, which
  2. additionhad been initially introduced into the reaction vessel
  3. stirringstirred thoroughly
  4. customThe product which precipitated
  5. filtrationwas filtered off
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-89f5f9d49d7f41f38de44e6c05b4f2eb
出典データセット
uspto-grants-1982_08
特許番号
US04345100

関連ノート

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