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

HRID 426356ノート

反応式

HRID 426356 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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

後処理

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

出典と根拠

ORDレコード
ord-a6e0258e68c945baacc58a9238da8512
出典データセット
uspto-grants-2012_01
特許番号
US08106236B2

反応ノート

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