Ammonia → 2-Methoxyphenyl-4-methylcyclohexanone

HRID 26482

반응식

HRID 26482 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.[NH2-].[Na+].Cl[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[O:18][CH3:19].N>O1CCCC1>[CH3:19][O:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[CH:4]1[CH2:3][CH:2]([CH3:1])[CH2:7][CH2:6][C:5]1=[O:8]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 115254-MethylcyclohexanoneHCID 130112-ChloroanisoleHCID 24533Sodium amide

생성물 1

HCID 213232862-Methoxyphenyl-4-methylcyclohexanone

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4-Methylcyclohexanone (224 g, 2 moles) was added dropwise rapidly to a cooled, stirred suspension of 170 g (4 moles) of sodium amide in 2 l of tetrahydrofuran under nitrogen. After the addition was complete, the ice bath was removed and the mixture was heated at reflux until the evolution of ammonia ceased (~3 hours). While still at reflux, 142.5 g (1 mole) of o-chloroanisole was added rapidly dropwise and the mixture was heated for an additional hour, until evolution of ammonia ceased.

후처리

  1. additionAfter the addition
  2. customthe ice bath was removed
  3. temperaturethe mixture was heated
  4. temperatureat reflux until the evolution of ammonia
  5. custom(~3 hours)
  6. temperatureWhile still at reflux

출처 및 근거

ORD 기록
ord-fac347d6f8b34305bb034a27a9abc60b
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150135

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