tert-Butanol → tert-Butyl (4-methylphenyl)acetate

HRID 636462

反応式

HRID 636462 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[CH:4][CH:3]=1.[C:12](O)([CH3:15])([CH3:14])[CH3:13].CN(C1C=CC=CN=1)C.C1(N=C=NC2CCCCC2)CCCCC1>ClCCl>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 6386tert-ButanolHCID 10868DicyclohexylcarbodiimideHCID 218852-DimethylaminopyridineHCID 248474p-Tolylacetic acid

生成物 1

HCID 12362014tert-Butyl (4-methylphenyl)acetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
25 °C

実験手順

450 g (3 mol) of 4-methylphenylacetic acid, 1.13 l (12 mol) of tert-butanol and 90 g (0.74 mol) of dimethylaminopyridine are dissolved in 2 l of dichloromethane. After addition of 680 g (3.3 mol) of dicyclohexylcarbodiimide, dissolved in 400 ml of dichloromethane, the mixture is stirred at 25° C. for 20 h, the precipitated urea is filtered off with suction and washed with 200 ml of dichloromethane, and the organic phase is washed twice each with 500 ml of 2M hydrochloric acid and water. The organic phase is dried using sodium sulphate, concentrated and distilled.

後処理

  1. filtrationthe precipitated urea is filtered off with suction
  2. washwashed with 200 ml of dichloromethane
  3. washthe organic phase is washed twice each with 500 ml of 2M hydrochloric acid and water
  4. customThe organic phase is dried
  5. concentrationconcentrated
  6. distillationdistilled

出典と根拠

ORDレコード
ord-3ea04fe0288045e8a8ddbb04ad8ed205
出典データセット
uspto-grants-2001_02
特許番号
US06194424B1

関連ノート

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