3-{2-Methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid → 2-Methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid

HRID 4752

反応式

HRID 4752 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([OH:18])([C:14]([F:17])([F:16])[F:15])[C:10]([F:13])([F:12])[F:11])[CH:6]=[CH:5][C:4]=1[CH:19]=[CH:20][C:21]([OH:23])=[O:22]>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([OH:18])([C:14]([F:15])([F:16])[F:17])[C:10]([F:13])([F:12])[F:11])[CH:6]=[CH:5][C:4]=1[CH2:19][CH2:20][C:21]([OH:23])=[O:22]

参加物

3

反応物 1

HCID 545552723-{2-Methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid

生成物 1

HCID 140766562-Methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid収率 80.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To 100 ml of ethanol are added 8.8 g (0.025 mole) of 3-{2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid to produce a solution which is added to a pressure bottle and flushed with nitrogen. To the solution is added 1 g of 10% palladium on carbon. The pressure bottle is placed in a hydrogenation apparatus and pressurized to 1384 g/cm2 (50 lbs/in.2) with hydrogen. The pressure bottle is shaken until the pressure ceases dropping. The resulting solution is vented, filtered and evaporated at reduced pressure to obtain a residual solid which is recrystallized from chlorobutane o give 7.0 gm of 2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid having a melting point of 116°-117°.

後処理

  1. customto produce a solution which
  2. additionis added to a pressure bottle
  3. customflushed with nitrogen
  4. additionTo the solution is added 1 g of 10% palladium on carbon
  5. filtrationfiltered
  6. customevaporated at reduced pressure
  7. customto obtain a residual solid which
  8. customis recrystallized from chlorobutane

出典と根拠

ORDレコード
ord-5311bd096d1c45b1920e980fa0c4e746
出典データセット
uspto-grants-1988_02
特許番号
US04727180

関連ノート

読み込み中…