Hydrogen Peroxide → HCID 18617845, 화합물

HRID 1078417노트

반응식

HRID 1078417 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 18617845HCID 18617845, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-45205572723d43a7bd373a9db1adab20
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05547972

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