Water → HCID 60026890、化合物

HRID 400626ノート

反応式

HRID 400626 の反応式
[F:1][C:2]([CH:4]([OH:16])[CH2:5][C:6]([C:9]1[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=1)([CH3:8])[CH3:7])=[CH2:3].[CH2:17]([Zn]CC)C.ICI.O>C(OCC)(=O)C>[F:1][C:2]1([CH:4]([OH:16])[CH2:5][C:6]([C:9]2[CH:10]=[CH:11][C:12]([F:15])=[CH:13][CH:14]=2)([CH3:8])[CH3:7])[CH2:17][CH2:3]1

参加物

6

反応物 4

HCID 962WaterHCID 6346DiiodomethaneHCID 600266962-Fluoro-5-(4-fluorophenyl)-5-methylhex-1-en-3-olHCID 178418750HCID 178418750、化合物

生成物 1

HCID 60026890HCID 60026890、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To the above crude 2-fluoro-5-(4-fluorophenyl)-5-methylhex-1-en-3-ol (1.73 g, 7.65 mmol) stirred under nitrogen gas and cooled on ice, was added diethyl zinc (1.1 M in toluene, 8.0 mL). After 5 minutes, 1.0 mL of diiodomethane was added dropwise over 20 minutes and the mixture was stirred and allowed to come to room temperature and then stirred at room temperature for 4 days. 0.5 mL of water was then added to the reaction mixture, followed by ethyl acetate. The resulting mixture was then filtered through diatomaceous earth and the solvent was removed in vacuo and the residue was fractionated over silica gel (hexanes-dichloromethane (1:1) to dichloromethane gradient) to give 1-(1-fluorocyclopropyl)-3-(4-fluorophenyl)-3-methylbutan-1-ol as an oil.

後処理

  1. temperaturecooled on ice
  2. customto come to room temperature
  3. stirringstirred at room temperature for 4 days
  4. filtrationThe resulting mixture was then filtered through diatomaceous earth
  5. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-1535e171f5ec4c55aa832806c599c3d4
出典データセット
uspto-grants-2014_06
特許番号
US08741897B2

反応ノート

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