Pyridine → 2-(3,5-Bis-trifluoromethanesulfonyloxy-phenyl)-4-methyl-pentanoic acid methyl ester

HRID 426356노트

반응식

HRID 426356 반응식
FC(F)(F)S([O:6][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:9])=[O:8])(=O)=O.[CH3:16][O:17][C:18](=[O:32])[CH:19]([C:24]1[CH:29]=[C:28]([OH:30])[CH:27]=[C:26](O)[CH:25]=1)[CH2:20][CH:21]([CH3:23])[CH3:22].N1C=CC=CC=1>C(Cl)Cl>[CH3:16][O:17][C:18](=[O:32])[CH:19]([C:24]1[CH:29]=[C:28]([O:30][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:8])=[O:6])[CH:27]=[C:26]([O:6][S:7]([C:10]([F:11])([F:12])[F:13])(=[O:8])=[O:9])[CH:25]=1)[CH2:20][CH:21]([CH3:23])[CH3:22]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 67749Trifluoromethanesulfonic anhydrideHCID 590047662-(3,5-Dihydroxy-phenyl)-4-methyl-pentanoic acid methyl ester

생성물 1

HCID 590047892-(3,5-Bis-trifluoromethanesulfonyloxy-phenyl)-4-methyl-pentanoic acid methyl ester수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoromethanesulfonic anhydride (208 μL, 1.26 mmol) was added dropwise to a stirred solution of 2-(3,5-dihydroxy-phenyl)-4-methyl-pentanoic acid methyl ester (50 mg, 0.21 mmol) and pyridine (195 μL, 2.52 mmol) in DCM (5 mL) at 0° C. then warmed to room temperature. After 1 h, the mixture washed with 1M HCl (2 mL), dried (MgSO4) and concentrated in vacuo to afford the title product as an orange oil (104 mg, 99%). The product was used without further purification in the next step

후처리

  1. washthe mixture washed with 1M HCl (2 mL)
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a6e0258e68c945baacc58a9238da8512
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106236B2

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