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Water → 1-(2-Methyl-2-phenylpropoxy)-4-nitrobenzene

HRID 1679504
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HRID 1679504 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7](Cl)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:11][C:12]([CH3:21])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:13][OH:14].[H-].[Na+].O>CS(C)=O>[CH3:11][C:12]([CH3:21])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH2:13][O:14][C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 74741-Chloro-4-nitrobenzeneHCID 24758Sodium hydrideHCID 219535beta,beta-Dimethylbenzeneethanol

생성물 1

HCID 128250041-(2-Methyl-2-phenylpropoxy)-4-nitrobenzene수율 72%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

In 200 ml of dimethylsulfoxide are dissolved 23 g of 4-nitrochlorobenzene and 25 g of 2,2-dimethyl-2-phenylethylalcohol. To this solution is added 4 g of sodium hydride is added with stirring. After 24 hours stirring at room temperature and another 30 minutes stirring at 60° C, 500 ml of water is added and the mixture is extracted with ether. The extract is washed with water, dried and the solvent is evaporated. Recrystallization of the residue from 200 ml of methanol, gives 28.5 g of 4-(2,2-dimethyl-2-phenylethyloxy)nitrobenzene, melting point: 79°-80° C.

후처리

  1. additionis added
  2. stirringAfter 24 hours stirring at room temperature and another 30 minutes
  3. stirringstirring at 60° C
  4. extractionthe mixture is extracted with ether
  5. washThe extract is washed with water
  6. customdried
  7. customthe solvent is evaporated
  8. customRecrystallization of the residue from 200 ml of methanol

출처 및 근거

ORD 기록
ord-a0a5b1197f904bc5a824d4b3fdd8d39f
출처 데이터셋
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04080505

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