반응 #3707

ord-1b59e09c326a4a03910529e081276b80

반응 방정식

COC(=O)c1ccc(CC(=O)c2ccccc2Cl)cc1
methyl 4-[2-(2-chlorophenyl)-2-oxoethyl]benzoate
[Na+].[OH-]
NaOH
O=C(O)CC(O)(CC(=O)O)C(=O)O
citric acid
O=C(O)c1ccc(CC(=O)c2ccccc2Cl)cc1
desired product
수율 96.7%
O=C(O)c1ccc(CC(=O)c2ccccc2Cl)cc1
4-[2-(2-Chlorophenyl)-2-oxoethyl]benzoic acid
수율 96.7%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is refluxed for 3 hours
  2. 2
    기타The reaction mixture is evaporated in vacuo
  3. 3
    기타to remove the CH3OH
  4. 4
    추출The aqueous phase is extracted with CH2Cl2
  5. 5
    기타The resulting solid is collected
  6. 6
    기타dried under vacuum

실험 절차

A mixture of 18.78 g of methyl 4-[2-(2-chlorophenyl)-2-oxoethyl]benzoate in 288.8 ml of CH3OH, 72.2 ml of water and 5.2 g of NaOH is refluxed for 3 hours then acidified with 2N citric acid. The reaction mixture is evaporated in vacuo to remove the CH3OH. The aqueous phase is extracted with CH2Cl2 and acidified with 1N HCl. The resulting solid is collected and dried under vacuum to give 17.27 g of the desired product, m.p. 168°-172° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733905uspto-grants-1998_03