Sodium Hydroxide → 2,6-Dichloro-alpha-methylenebenzene propanoic acid

HRID 1904582노트

반응식

HRID 1904582 반응식
[OH-].[Na+].[I-].[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:6]=1[CH2:12][CH:13]([C:19]([O:21]C)=[O:20])[CH2:14][N+](C)(C)C>CO>[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[C:6]=1[CH2:12][C:13](=[CH2:14])[C:19]([OH:21])=[O:20]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 20037664HCID 20037664, 화합물

생성물 1

HCID 867431352,6-Dichloro-alpha-methylenebenzene propanoic acid수율 112.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Under an inert atmosphere, 120 ml of 2N sodium hydroxide were added to 53.3 g of the product of Step B in suspension in 500 ml of methanol. After refluxing the mixture for 2 hours, the solvents were eliminated under reduced pressure, and the residual aqueous phase was extracted with ether. After acidifying with 5N hydrochloric acid, extraction was done again with ether and then with ethyl acetate. The combined organic phases were dried, and the solvents were eliminated under reduced pressure to obtain 32 g of crude product which was crystallized from hexane and then melted at 132° C.

후처리

  1. temperatureAfter refluxing the mixture for 2 hours
  2. extractionthe residual aqueous phase was extracted with ether
  3. extractionAfter acidifying with 5N hydrochloric acid, extraction
  4. customThe combined organic phases were dried

출처 및 근거

ORD 기록
ord-8603bd97639043758527e18c93b0f839
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839358

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