Ethanol → Diethyl 2,2'-(1,3-phenylene)diacetate

HRID 499848

반응식

HRID 499848 반응식
[C:1](Cl)(=O)[CH3:2].[C:5]1([CH2:15][C:16]([OH:18])=[O:17])[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][C:12]([OH:14])=[O:13])[CH:6]=1.[CH2:19](O)[CH3:20]>>[C:5]1([CH2:15][C:16]([O:18][CH2:1][CH3:2])=[O:17])[CH:10]=[CH:9][CH:8]=[C:7]([CH2:11][C:12]([O:14][CH2:19][CH3:20])=[O:13])[CH:6]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 6367Acetyl chlorideHCID 29788m-Phenylenediacetic acid

생성물 1

HCID 19863769Diethyl 2,2'-(1,3-phenylene)diacetate

실험 절차

Acetyl chloride (12.5 ml, 175 mmol) was added to a suspension of 2,2′-(1,3-phenylene)diacetic acid (50.0 g, 260 mmol) in ethanol (500 ml) and the resulting solution heated to reflux for 16 hours. The reaction was cooled to room temperature and the solvent removed in vacuo. The residue was partitioned between saturated aqueous sodium hydrogencarbonate (300 ml) and ethyl acetate (500 ml). The organic phase was washed with water (200 ml). sat. aq. sodium chloride (300 ml), dried (sodium sulfate) and the solvent removed in vacuo to give the title compound as a pale yellow oil (63.5 g).

후처리

  1. temperaturethe resulting solution heated
  2. temperatureto reflux for 16 hours
  3. customthe solvent removed in vacuo
  4. customThe residue was partitioned between saturated aqueous sodium hydrogencarbonate (300 ml) and ethyl acetate (500 ml)
  5. washThe organic phase was washed with water (200 ml)
  6. dry with materialsat. aq. sodium chloride (300 ml), dried (sodium sulfate)
  7. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-b320b2d5d87944599f49c91ebb360659
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767715B2

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