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

HRID 494415ノート

反応式

HRID 494415 の反応式
[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

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

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.

後処理

  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

出典と根拠

ORDレコード
ord-9bd19ea7716141d087555c03aeb06612
出典データセット
uspto-grants-2009_05
特許番号
US07538141B2

反応ノート

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