Ethanol → Ethyl (2-chlorobenzoyl)acetate

HRID 986231

反応式

HRID 986231 の反応式
[H-].[Na+].[C:3](=[O:10])([O:7][CH2:8][CH3:9])OCC.[Cl:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18](=[O:20])[CH3:19].C(O)C>O1CCCC1>[Cl:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[C:18]([CH2:19][C:3]([O:7][CH2:8][CH3:9])=[O:10])=[O:20]

参加物

6

反応物 4

HCID 702Ethanol2 回HCID 7766Diethyl CarbonateHCID 24758Sodium hydrideHCID 72864Ethanone, 1-(2-chlorophenyl)-

生成物 1

HCID 292405Ethyl (2-chlorobenzoyl)acetate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Sodium hydride (8.7 grams) and 21.4 grams of diethyl carbonate are suspended in 100 ml of tetrahydrofuran, 14 grams of o-chloroacetophenone is gradually dropped thereinto by keeping the inner temperature at 40° to 50° C., then a small amount of ethanol is added thereto and heated to reflux for four hours. After cooling, 20 ml of ethanol is added thereto, the mixture is poured into ice water, and extracted with ether. Ether extracts are combined, washed with water, dried with anhydrous magnesium sulfate, and ether is evaporated therefrom. The resulting oil is purified by distillation in vacuo to give 8.8 grams of colorless, oily product, b.p. 120° to 125° C./1 mmg Hg.

後処理

  1. customat 40° to 50° C.
  2. temperatureheated
  3. temperatureto reflux for four hours
  4. temperatureAfter cooling
  5. extractionextracted with ether
  6. washwashed with water
  7. dry with materialdried with anhydrous magnesium sulfate, and ether
  8. customis evaporated
  9. distillationThe resulting oil is purified by distillation in vacuo
  10. customto give 8.8 grams of colorless, oily product, b.p. 120° to 125° C./1 mmg Hg

出典と根拠

ORDレコード
ord-3823c647e0a742aa85112ba7366a48a0
出典データセット
uspto-grants-1987_12
特許番号
US04711898

関連ノート

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