Sodium Hydroxide → HCID 22010353, 화합물

HRID 322894노트

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HRID 322894 반응식
[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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 54430731HCID 54430731, 화합물

생성물 1

HCID 22010353HCID 22010353, 화합물수율 83.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%].

후처리

  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

출처 및 근거

ORD 기록
ord-0e23a8182da7481db4676d2021657941
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211234B1

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