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

HRID 499848ノート

反応式

HRID 499848 の反応式
[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

参加物

4

反応物 3

HCID 702EthanolHCID 6367Acetyl chlorideHCID 29788m-Phenylenediacetic acid

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b320b2d5d87944599f49c91ebb360659
出典データセット
uspto-grants-2010_08
特許番号
US07767715B2

反応ノート

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