홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Sodium hydride → (RS)-5-[2-cyano-5-(3-thienylmethoxy)phenoxy]-5-(2-methylphenyl)pentanoic acid

HRID 322907
노트
인쇄 미리보기

반응식

HRID 322907 반응식
[H-].[Na+].[OH:3][CH:4]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[CH3:17])[CH2:5][CH2:6][CH2:7][C:8]([O-:10])=[O:9].[Na+].F[C:20]1[CH:27]=[C:26]([O:28][CH2:29][C:30]2[CH:34]=[CH:33][S:32][CH:31]=2)[CH:25]=[CH:24][C:21]=1[C:22]#[N:23]>O1CCCC1>[C:22]([C:21]1[CH:24]=[CH:25][C:26]([O:28][CH2:29][C:30]2[CH:34]=[CH:33][S:32][CH:31]=2)=[CH:27][C:20]=1[O:3][CH:4]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[CH3:17])[CH2:5][CH2:6][CH2:7][C:8]([OH:10])=[O:9])#[N:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 107283302-Fluoro-4-(3-thienylmethoxy)benzonitrileHCID 86756591sodium (RS)-5-hydroxy-5-(2-methylphenyl)pentanoate

생성물 1

HCID 22010371(RS)-5-[2-cyano-5-(3-thienylmethoxy)phenoxy]-5-(2-methylphenyl)pentanoic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
57.5 °C

실험 절차

To a stirred suspension of sodium hydride (0.69 g, 60% dispersion in mineral oil) in dry tetrahydrofuran (50 mL) is added a solution of sodium (RS)-5-hydroxy-5-(2-methylphenyl)pentanoate (1.23 g) in dry tetrahydrofuran (100 mL). The mixture is stirred at room temperature for 1.5 hours when 2-fluoro-4-(3-thienylmethoxy)benzonitrile (1.57 g) is added in one portion. The reaction mixture is heated at 55-60° C. for 18 hours and evaporated. The residue is dissolved in water (100 mL), the solution acidified to pH 1 with 1 N hydrochloric acid and the mixture extracted three times with ethyl acetate (100 mL). The combined extracts are washed with brine (100 mL), dried over magnesium sulphate and evaporated to give (RS)-5-[2-cyano-5-(3-thienylmethoxy)phenoxy]-5-(2-methylphenyl)pentanoic acid as a white waxy solid (0.4 g), mp.p.106-108° C. [Elemental analysis:- C,67.15; H,5.84; N,2.75; S,6.99%. Calculated for C24H23NO4S.0.5EtOAc:- C,66.66; H,4.66; N,6.48%].

후처리

  1. additionis added in one portion
  2. customevaporated
  3. dissolutionThe residue is dissolved in water (100 mL)
  4. extractionthe mixture extracted three times with ethyl acetate (100 mL)
  5. washThe combined extracts are washed with brine (100 mL)
  6. dry with materialdried over magnesium sulphate
  7. customevaporated

출처 및 근거

ORD 기록
ord-e5a75c5bb54847a3a3d45b1855dacd4b
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06211234B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트