Sodium Hydroxide → 2-(3-Chloro-4-(methylsulfonyl)phenyl)propanoic acid

HRID 1843014ノート

反応式

HRID 1843014 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]([CH3:17])[C:13]([O:15]C)=[O:14])[CH:5]=[CH:6][C:7]=1[S:8]([CH3:11])(=[O:10])=[O:9].[OH-].[Na+].C(OCC)(=O)C.CCCCCC>CO.O.Cl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]([CH3:17])[C:13]([OH:15])=[O:14])[CH:5]=[CH:6][C:7]=1[S:8]([CH3:11])(=[O:10])=[O:9]

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 21226206Ethyl acetate hexaneHCID 70816425Methyl 2-(3-chloro-4-(methylsulfonyl)phenyl)propanoate

生成物 1

HCID 583693082-(3-Chloro-4-(methylsulfonyl)phenyl)propanoic acid収率 88.9%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒2 回HCID 962Water溶媒2 回

実験手順

To a solution of methyl 2-(3-chloro-4-(methylsulfonyl)phenyl)propanoate (3.2 g, crude) in methanol (32 mL, 10 times), a solution of sodium hydroxide (0.46 g, 1 eq) in water (5 mL) was added at 0° C. The contents were warmed to room temperature and allowed to stir for 2 h. Progress of the reaction was monitored by TLC (50% ethyl acetate/hexane, Rf˜0.1). On completion of the reaction, methanol was distilled off completely and the residue obtained was taken in water. The contents were acidified to a pH of 4 and diluted with HCl at 0° C., the precipitate was filtered and dried to yield 2-(3-chloro-4-(methylsulfonyl)phenyl)propanoic acid as a white colored solid (2.7 g, 88%).

後処理

  1. distillationwas distilled off completely
  2. customthe residue obtained
  3. filtrationthe precipitate was filtered
  4. customdried

出典と根拠

ORDレコード
ord-1fea35f1a1524651b907879ae3020a1b
出典データセット
uspto-grants-2015_02
特許番号
US08946204B2

反応ノート

読み込み中…