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HCID 19005115、化合物 → HCID 19005118、化合物

HRID 1762783
ノート
印刷プレビュー

反応式

HRID 1762783 の反応式
O=C1[CH:6]([C:7](=[O:17])[C:8]([F:16])([F:15])[CH2:9][CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:5][CH2:4][O:3]1>Cl.C(O)(=O)C>[OH:3][CH2:4][CH2:5][CH2:6][C:7](=[O:17])[C:8]([F:16])([F:15])[CH2:9][CH2:10][C:11]([CH3:12])([CH3:13])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 19005115HCID 19005115、化合物

生成物 1

HCID 19005118HCID 19005118、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 176Acetic Acid溶媒

実験手順

A 10 mL one neck round bottom flask, fitted with argon inlet, magnetic stirrer, and reflux condenser was charged with 1.0 mL glacial acetic acid, 4 drops of concentrated HCl and 200 mg (0.81 mM) of 2,3,4,5-tetrahydro-2-oxo-3-(5,5-dimethyl-2,2-difluoro-1-oxohexyl)furan. The reaction mixture was heated at 110 C. overnight under a blanket of argon. The reaction was extracted with ethyl ether, and the ether was cross washed with water, dried (anhydrous MgSO4), and solvent removed under reduced pressure. The residue was chromatographed on a 10×60 mm silica gel column using a 9:1 hexane:ethyl acetate mixture to give a clear oil. nmr(CDCl3)--α0.95(s, 9H), 1.45(t, 2H), 2.00(m, 6H), 3.12(bs, 1H), 4.15(m, 1H)

後処理

  1. temperaturereflux condenser
  2. temperatureThe reaction mixture was heated at 110 C
  3. customovernight
  4. extractionThe reaction was extracted with ethyl ether
  5. washthe ether was cross washed with water
  6. dry with materialdried (anhydrous MgSO4), and solvent
  7. customremoved under reduced pressure
  8. customThe residue was chromatographed on a 10×60 mm silica gel column
  9. customethyl acetate mixture to give a clear oil

出典と根拠

ORDレコード
ord-d4b9516a6e524e438aa0e9e52fcc9f95
出典データセット
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04835099

反応ノート

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