Water → HCID 57736276、化合物

HRID 2261327ノート

反応式

HRID 2261327 の反応式
F[C:2](F)([C:10]([F:13])([F:12])[F:11])[CH:3]=[C:4](I)[CH:5]([OH:8])[CH2:6][CH3:7].[OH2:15].Cl.[NH2:17]O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:11][C:10]([F:13])([F:12])[C:2]1[O:15][N:17]=[C:4]([CH:5]([OH:8])[CH2:6][CH3:7])[CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 86631046HCID 86631046、化合物

生成物 1

HCID 57736276HCID 57736276、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

9.01 g of 6,6,7,7,7-pentafluoro-4-iodo-4-heptene-3-ol was dissolved in 70 ml of ethanol, and 30 ml of water, 3.81 g of hydroxylamine hydrochloride and 7.51 g of potassium carbonate were then added. The mixture was stirred and heated under reflux for 24 hours. The reaction mixture was concentrated under reduced pressure. After water was added, the residue was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 1.63 g of 1-(5-trifluoromethyl-isoxazol-3-yl)propanol.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 24 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionAfter water was added
  5. extractionthe residue was extracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-62bcf74ae3184c99b772731b0ed353bc
出典データセット
uspto-grants-2010_12
特許番号
US07846956B2

反応ノート

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