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

HRID 1904582ノート

反応式

HRID 1904582 の反応式
[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]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 20037664HCID 20037664、化合物

生成物 1

HCID 867431352,6-Dichloro-alpha-methylenebenzene propanoic acid収率 112.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8603bd97639043758527e18c93b0f839
出典データセット
uspto-grants-1989_06
特許番号
US04839358

反応ノート

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