Trifluoroacetic acid → HCID 13356241、化合物

HRID 660283ノート

反応式

HRID 660283 の反応式
COC[O:4][C:5]1[CH:6]=[C:7]([CH:11]([CH3:17])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:8]=[CH:9][CH:10]=1.FC(F)(F)C(O)=O.C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[OH:4][C:5]1[CH:6]=[C:7]([CH:11]([CH3:17])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:8]=[CH:9][CH:10]=1

参加物

6

反応物 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 57742132HCID 57742132、化合物

生成物 1

HCID 13356241HCID 13356241、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A solution of Ethyl 2-(3-(methoxymethoxy)phenyl)propanoate (4.17 g, 17.5 mmol) in CH2Cl2 (80 mL) was added trifluoroacetic acid (40 mL) at 0° C. The reaction mixture was stirred for 1 hrs at 0° C., and basified with NaHCO3 (60 g). The mixture was diluted with H2O (250 mL) slowly and extracted with CH2Cl2. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using EtOAc:hexanes (1:4) as eluant.

後処理

  1. extractionextracted with CH2Cl2
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash column chromatography on silica gel

出典と根拠

ORDレコード
ord-8c92c2437e134961b65aa962fd05d231
出典データセット
uspto-grants-2011_12
特許番号
US08084484B2

反応ノート

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