Hydrochloric Acid → 1-(2,4-Dimethyl-5-oxazolyl)-1-(3-furyl)-2,2,2-trifluoroethanol

HRID 975073

反応式

HRID 975073 の反応式
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[O:19]1[CH:23]=[CH:22][C:21]([C:24]([C:26]2[O:30][C:29]([CH3:31])=[N:28][C:27]=2[CH3:32])=[O:25])=[CH:20]1.[F:33][C:34]([Si](C)(C)C)([F:36])[F:35].Cl.C(=O)([O-])O.[Na+]>O1CCCC1>[CH3:31][C:29]1[O:30][C:26]([C:24]([C:21]2[CH:22]=[CH:23][O:19][CH:20]=2)([OH:25])[C:34]([F:36])([F:35])[F:33])=[C:27]([CH3:32])[N:28]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 552549(Trifluoromethyl)trimethylsilaneHCID 2724141Tetrabutylammonium FluorideHCID 537121082,4-Dimethyl-5-oxazolyl 3-furyl ketone

生成物 1

HCID 189363371-(2,4-Dimethyl-5-oxazolyl)-1-(3-furyl)-2,2,2-trifluoroethanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Tetrabutylammonium fluoride (250 mg) was added to a stirred solution of 2,4-dimethyl-5-oxazolyl 3-furyl ketone (1.7 g) and (trifluoromethyl)trimethylsilane (1.9 g) in dry tetrahydrofuran (30 ml) at -10° C. The mixture was allowed to warm to room temperature. After 45 minutes 6M hydrochloric acid (30 ml) was added. After 1 hour the mixture was basified by the addition of saturated aqueous sodium hydrogen carbonate and then extracted with dichloromethane. The material thus obtained was purified by flash chromatography and recrystallisation from diethyl ether.

後処理

  1. extractionextracted with dichloromethane
  2. customThe material thus obtained
  3. customwas purified by flash chromatography and recrystallisation from diethyl ether

出典と根拠

ORDレコード
ord-e04629eb18754e708625eb016629151c
出典データセット
uspto-grants-1997_03
特許番号
US05607956

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