Hydrogen Peroxide → HCID 18617845、化合物

HRID 1078417ノート

反応式

HRID 1078417 の反応式
[C:1]([C:3]([C:6]1[CH:15]=[CH:14][C:9]([C:10]([O:12]C)=[O:11])=[CH:8][CH:7]=1)([CH3:5])[CH3:4])#[N:2].[OH-:16].[Na+].OO>O>[C:1]([C:3]([C:6]1[CH:15]=[CH:14][C:9]([C:10]([OH:12])=[O:11])=[CH:8][CH:7]=1)([CH3:5])[CH3:4])(=[O:16])[NH2:2]

参加物

5

反応物 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 14698604Methyl 4-(1-cyano-1-methylethyl)benzoate

生成物 1

HCID 18617845HCID 18617845、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

A mixture of methyl 4-(1-cyano-1-methylethyl)benzoate (1.0 g), sodium hydroxide (0.4 g), water (2 ml) and IMS (5 ml) was heated to 50° C. with stirring. Hydrogen peroxide (60% w/v, 1.23 ml) was added dropwise and the reaction mixture was stirred at 50° C. for 1 hour. and then at ambient temperature for 3 hours. The reaction mixture was evaporated to dryness under reduced pressure. Water (10 ml) was added to the residue and this mixture was heated at 95° C. for 1 hour. The mixture was cooled, washed with dichloromethane, acidified with 5M hydrochloric acid and filtered to give 4-(1-carbamoyl-1-methylethyl)benzoic acid, m.p. 218°-219° C.

後処理

  1. stirringthe reaction mixture was stirred at 50° C. for 1 hour
  2. customThe reaction mixture was evaporated to dryness under reduced pressure
  3. additionWater (10 ml) was added to the residue
  4. temperaturethis mixture was heated at 95° C. for 1 hour
  5. temperatureThe mixture was cooled
  6. washwashed with dichloromethane
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-45205572723d43a7bd373a9db1adab20
出典データセット
uspto-grants-1996_08
特許番号
US05547972

反応ノート

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