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

HRID 1679504
ノート
印刷プレビュー

反応式

HRID 1679504 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 128250041-(2-Methyl-2-phenylpropoxy)-4-nitrobenzene収率 72%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a0a5b1197f904bc5a824d4b3fdd8d39f
出典データセット
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04080505

反応ノート

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