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

HRID 25152

反応式

HRID 25152 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].C1(N=C=NC2CCCCC2)CCCCC1>CN(C1C=CN=CC=1)C.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 3

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

生成物 1

HCID 12362014tert-Butyl (4-methylphenyl)acetate

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
25 °C

実験手順

450 g (3 mol) of 4-methylphenyl-acetic acid (Aldrich), 1.13 l (12 mol) of tert-butanol and 90 g (0.74 mol) of 4-(N,N-dimethylamino)pyridine 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 flashed with 200 ml of dichloromethane, and the organic phase is washed twice each with 500 ml of 2 M hydrochloric acid and water. The organic phase is concentrated and distilled.

後処理

  1. filtrationthe precipitated urea is filtered off with suction
  2. washthe organic phase is washed twice each with 500 ml of 2 M hydrochloric acid and water
  3. concentrationThe organic phase is concentrated
  4. distillationdistilled

出典と根拠

ORDレコード
ord-d11bec94770c4b5c9e1b124727c52863
出典データセット
uspto-grants-2005_02
特許番号
US06858622B2

関連ノート

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