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Trifluoroacetic acid → 4-(4-Chlorophenyl)-5-methoxy-4-methyl-5-oxopentanoic acid

HRID 82377
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HRID 82377 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:22])([CH2:13][CH2:14][C:15]([O:17]C(C)(C)C)=[O:16])[C:9]([O:11][CH3:12])=[O:10])=[CH:4][CH:3]=1.C(O)(C(F)(F)F)=O>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:22])([C:9]([O:11][CH3:12])=[O:10])[CH2:13][CH2:14][C:15]([OH:17])=[O:16])=[CH:4][CH:3]=1
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참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 673381775-Tert-butyl 1-methyl 2-(4-chlorophenyl)-2-methylpentanedioate

생성물 1

HCID 673392784-(4-Chlorophenyl)-5-methoxy-4-methyl-5-oxopentanoic acid수율 101.5%

실험 절차

Methyl 2-(4-chlorophenyl)propanoate (1.50 g, 7.55 mmol) was dissolved in THF (14 mL) and cooled to 0° C. The solution was treated with KOtBu (85 mg, 0.755 mmol) and allowed to stir for 15 minutes. The solution was cooled to −78° C. and then treated with the acrylate (1.22 mL, 8.31 mmol). The mixture was allowed to stir overnight to room temperature to completion by TLC analysis. The mixture was then quenched with saturated NH4Cl. The THF was removed in vacuo to afford a yellow oil. The residue was partitioned between ethyl acetate and water. The aqueous was extracted with ethyl acetate, and the organics were combined. The organic portion was washed with water, then brine, separated, dried over MgSO4, filtered, and concentrated in vacuo to afford the crude material as a yellow oil. The material was purified by chromatography (silica gel eluted with 90:10 hexanes:ethyl acetate, Rf=0.35) to afford 5-tert-butyl 1-methyl 2-(4-chlorophenyl)-2-methylpentanedioate as a colorless oil (1.69 g, 69%). This 5-tert-butyl 1-methyl 2-(4-chlorophenyl)-2-methylpentanedioate (1.69 g, 5.17 mmol) was dissolved in TFA (15.9 mL; 207 mmol) at room temperature and allowed to stir for 2 hours to completion by LCMS (neg) analysis. The solution was concentrated in vacuo to afford 4-(4-chlorophenyl)-5-methoxy-4-methyl-5-oxopentanoic acid as a colorless oil (1.42 g, 100%).

후처리

  1. concentrationThe solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-ada9d4edbb5644a693e8d069e2b93f87
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846681B2

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