Trifluoroacetic acid → 2,3-Dihydro-6-hydroxy-3-phenylinden-1-one

HRID 331260ノート

反応式

HRID 331260 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:8](=[O:17])/[CH:9]=[CH:10]/[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:5]=[CH:6][CH:7]=1.C(O)(C(F)(F)F)=O>C1(C)C=CC=CC=1>[OH:1][C:2]1[CH:3]=[C:4]2[C:5]([CH:10]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:9][C:8]2=[O:17])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 5356382T5637827

生成物 1

HCID 703075012,3-Dihydro-6-hydroxy-3-phenylinden-1-one収率 99%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

(E)-1-(3-Hydroxyphenyl)-3-phenylprop-2-en-1-one (48.7 g, 217 mmol) obtained in Step 1 and CF3COOH (161 mL, 10 eq) were placed into a flask and stirred for 24 h at 80° C. After cooling to room temperature, toluene (200 mL) was added and the solution was concentrated to remove TFA under reduced pressure. The residue was dissolved in EtOAc, washed with H2O, dried over MgSO4, and concentrated in vacuo to obtain the desired product (48.0 g, 99%).

後処理

  1. temperatureAfter cooling to room temperature
  2. concentrationthe solution was concentrated
  3. customto remove TFA under reduced pressure
  4. dissolutionThe residue was dissolved in EtOAc
  5. washwashed with H2O
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c6278b364d5449678b2c237d922c7ead
出典データセット
uspto-grants-2014_11
特許番号
US08877747B2

反応ノート

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