Sulfuric Acid → phenylglyoxylic-N-t-butylamide

HRID 27837

反応式

HRID 27837 の反応式
[C:1]([C:9]#[N:10])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:11](O)([CH3:14])([CH3:13])[CH3:12].S(=O)(=O)(O)[OH:17]>C(Cl)Cl>[C:11]([NH:10][C:9](=[O:17])[C:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:8])([CH3:14])([CH3:13])[CH3:12]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 6386tert-ButanolHCID 11953Phenylglyoxylonitrile

生成物 1

HCID 10965642phenylglyoxylic-N-t-butylamide収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

There were present in a stirrer equipped apparatus protected against moisture, 131 grams (1.0 mole) of benzoyl cyanide, 148 grams (2.0 moles) of t-butanol and 50 ml of methylene chloride and under stirring at about +50° C. it was treated by dropwise addition 150 grams (1.5 moles) of concentrated sulfuric acid. After the end of the dropping, the mixture was post-stirred for another hour at room temperature and then the entire mixture poured on 400 grams of ice and well agitated. Subsequently, the mixture was extracted with methylene chloride and the methylene chloride solution evaporated. There resulted 195 grams of phenylglyoxylic-N-t-butylamide which corresponds to a yield of 95% based on the acyl cyanide added. The amide has a melting point of 76°-77° C.

後処理

  1. customThere were present in a stirrer
  2. customequipped apparatus
  3. stirringAfter the end of the dropping, the mixture was post-stirred for another hour at room temperature
  4. stirringwell agitated
  5. extractionSubsequently, the mixture was extracted with methylene chloride
  6. customthe methylene chloride solution evaporated

出典と根拠

ORDレコード
ord-a22ed781f8d94aa9973b3334642eb21a
出典データセット
uspto-grants-1980_09
特許番号
US04224226

関連ノート

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