Sodium Hydroxide → HCID 22010353、化合物

HRID 322894ノート

反応式

HRID 322894 の反応式
[C:1]([C:4]([C:6]1[CH:27]=[CH:26][C:25]([O:28][CH2:29][C:30]2[CH:34]=[CH:33][S:32][CH:31]=2)=[CH:24][C:7]=1[O:8][CH:9]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH3:23])[CH2:10][CH2:11][C:12]([O:14]CC)=[O:13])=[O:5])([OH:3])=[O:2].[OH-].[Na+]>O1CCOCC1>[C:1]([C:4]([C:6]1[CH:27]=[CH:26][C:25]([O:28][CH2:29][C:30]2[CH:34]=[CH:33][S:32][CH:31]=2)=[CH:24][C:7]=1[O:8][CH:9]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[CH3:23])[CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:5])([OH:3])=[O:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 54430731HCID 54430731、化合物

生成物 1

HCID 22010353HCID 22010353、化合物収率 83.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A stirred solution of ethyl (RS)-4-(2-carboxycarbonyl-5-(3-thienylmethoxy)phenoxy)-4-(2-methylphenyl)butanoate (0.37 g) and 1 N sodium hydroxide (2.7 mL) in dioxan (6.6 mL) is heated at 60° C. for 1.5 hours. The reaction mixture is evaporated and the residue dissolved in water (5 mL). The pH of the solution is adjusted to 1 by addition of 1 N hydrochloric acid and the mixture extracted with ethyl acetate (20 mL). The organic phase is dried over magnesium sulphate and evaporated. The residual yellow oil is triturated with ether to give (RS)-4-(2-Carboxycarbonyl-5-(3-thienylmethoxy)phenoxy)-4-(2-methylphenyl)butanoic acid as a yellow solid (0.29 g), m.p. 173-175° C. [Elemental analysis:- C,63.2; H,5.07%. Calculated:- C,63.4; H,4.88%].

後処理

  1. customThe reaction mixture is evaporated
  2. dissolutionthe residue dissolved in water (5 mL)
  3. additionThe pH of the solution is adjusted to 1 by addition of 1 N hydrochloric acid
  4. extractionthe mixture extracted with ethyl acetate (20 mL)
  5. dry with materialThe organic phase is dried over magnesium sulphate
  6. customevaporated
  7. customThe residual yellow oil is triturated with ether

出典と根拠

ORDレコード
ord-0e23a8182da7481db4676d2021657941
出典データセット
uspto-grants-2001_04
特許番号
US06211234B1

反応ノート

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