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

HRID 494415노트

반응식

HRID 494415 반응식
[C:1]1([CH2:11][C:12]([OH:14])=[O:13])[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]([OH:10])=[O:9])[CH:2]=1.[C:15](Cl)(=O)[CH3:16].[CH2:19](O)[CH3:20]>>[C:1]1([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]([O:10][CH2:19][CH3:20])=[O:9])[CH:2]=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

2,2′-(1,3-Phenylene)diacetic acid (10.0 g, 51 mmol) was dissolved in ethanol (100 mL) and the solution treated dropwise with catalytic acetyl chloride (2.5 mL). The reaction mixture was stirred at reflux for 18 hours before being allowed to cool and concentrated under reduced pressure. The residue was taken up in ethyl acetate (100 mL) and washed with sodium bicarbonate solution (3×50 mL) and brine (3×50 mL). The organic phase was dried over magnesium sulphate and concentrated under reduced pressure. The residue was triturated with pentane to yield the title product, 11.8 g.

후처리

  1. temperatureat reflux for 18 hours
  2. temperatureto cool
  3. concentrationconcentrated under reduced pressure
  4. washwashed with sodium bicarbonate solution (3×50 mL) and brine (3×50 mL)
  5. dry with materialThe organic phase was dried over magnesium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was triturated with pentane

출처 및 근거

ORD 기록
ord-9bd19ea7716141d087555c03aeb06612
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538141B2

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