Ammonium Chloride → 2-Methyl-1-(3-trifluoromethyl-phenyl)-propan-2-ol

HRID 1295599

反応式

HRID 1295599 の反応式
[CH3:1][Mg]Br.[F:4][C:5]([F:17])([F:16])[C:6]1[CH:7]=[C:8]([CH2:12][C:13](=[O:15])[CH3:14])[CH:9]=[CH:10][CH:11]=1.[Cl-].[NH4+]>C(OCC)C.C1COCC1>[CH3:14][C:13]([OH:15])([CH3:1])[CH2:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([C:5]([F:16])([F:17])[F:4])[CH:7]=1

参加物

6

反応物 3

HCID 25517Ammonium ChlorideHCID 891011-(alpha,alpha,alpha-Trifluoro-m-tolyl)acetoneHCID 178418573HCID 178418573、化合物

生成物 1

HCID 149749932-Methyl-1-(3-trifluoromethyl-phenyl)-propan-2-ol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-50 °C

実験手順

90 mL of a 3 molar solution of methylmagnesium bromide in diethyl ether are diluted with 300 mL THF and cooled to −50° C. At this temperature 20 g 1-(3-trifluoromethyl-phenyl)-propan-2-one, dissolved in 100 mL THF, are added dropwise. After the addition has ended the reaction mixture is stirred overnight while heating to ambient temperature. It is combined with ammonium chloride solution and extracted with diethyl ether. The combined organic phases are washed with sodium chloride solution, dried with sodium sulphate and evaporated down. The residue remaining is purified by chromatography.

後処理

  1. additionare added dropwise
  2. additionAfter the addition
  3. temperaturewhile heating to ambient temperature
  4. extractionextracted with diethyl ether
  5. washThe combined organic phases are washed with sodium chloride solution
  6. dry with materialdried with sodium sulphate
  7. customevaporated down
  8. customThe residue remaining is purified by chromatography

出典と根拠

ORDレコード
ord-2a031326e45f4a968da9f97965d6ff33
出典データセット
uspto-grants-2007_07
特許番号
US07244728B2

関連ノート

読み込み中…