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

HRID 636462

반응식

HRID 636462 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 12362014tert-Butyl (4-methylphenyl)acetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ea04fe0288045e8a8ddbb04ad8ed205
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194424B1

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