Methyl iodide → 2,2-Dimethylcyclohexan-1-one

HRID 12032

反応式

HRID 12032 の反応式
[H-].[K+].[CH3:3][CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1=[O:10].[CH2:11](B(CC)CC)C.CI>O1CCCC1>[CH3:3][C:4]1([CH3:11])[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1=[O:10]

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 7357TriethylboraneHCID 114192-MethylcyclohexanoneHCID 82127Potassium hydride

生成物 1

HCID 1369292,2-Dimethylcyclohexan-1-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of potassium hydride (5.5 mmol) and 2-methylcyclohexanone (5 mmol) in dry tetrahydrofuran (10 ml) is stirred for 30 mins at room temperature. Triethylborane (6.25 mmol) is slowly added dropwise and the mixture is stirred for 16 hours at room temperature. After addition of methyl iodide stirring is continued for another 8 hours, the reaction is then quenched with saturated aqueous ammonium chloride solution and twice extracted with diethyl ether. The combined organic phases are dried over sodium sulphate and concentrated to dryness in a vacuum and produce the title compound, which can be reacted without [without] purification (JACS 1985, 107, 19, 5391-5396).

後処理

  1. stirringthe mixture is stirred for 16 hours at room temperature
  2. waitis continued for another 8 hours
  3. customthe reaction is then quenched with saturated aqueous ammonium chloride solution
  4. extractiontwice extracted with diethyl ether
  5. dry with materialThe combined organic phases are dried over sodium sulphate
  6. concentrationconcentrated to dryness in a vacuum

出典と根拠

ORDレコード
ord-86101b2e7f9945179d50d853ef03d403
出典データセット
uspto-grants-2010_06
特許番号
US07727979B2

関連ノート

読み込み中…