Ethanol → Ethyl (2-chlorobenzoyl)acetate

HRID 986231

반응식

HRID 986231 반응식
[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]

참가 물질

6

반응물 4

HCID 702Ethanol2회HCID 7766Diethyl CarbonateHCID 24758Sodium hydrideHCID 72864Ethanone, 1-(2-chlorophenyl)-

생성물 1

HCID 292405Ethyl (2-chlorobenzoyl)acetate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3823c647e0a742aa85112ba7366a48a0
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04711898

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