Water → HCID 13356241、化合物

HRID 660310ノート

反応式

HRID 660310 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+].O>C(Cl)Cl>[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 4

HCID 962WaterHCID 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 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

Ethyl 2-(3-(methoxymethoxy)phenyl)propanoate (4.17 g, 17.5 mmol) in methylene chloride (80 mL) was added trifluoroacetic acid (40 mL) at 0° C. The mixture was stirred for 1 hr at 0° C. and then slowly added solid sodium bicarbonate (60 g) and water (250 mL) at 0° C. The mixture was extracted with methylene chloride. The organic layer was dried with MgSO4. The organic layer was filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography eluting with n-Hexane/EtOAc=4/1.

後処理

  1. customat 0° C
  2. extractionThe mixture was extracted with methylene chloride
  3. dry with materialThe organic layer was dried with MgSO4
  4. filtrationThe organic layer was filtered
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe residue was purified by column chromatography
  7. washeluting with n-Hexane/EtOAc=4/1

出典と根拠

ORDレコード
ord-91a4c765d45b4501814b1edc5a8e6017
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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