반응 #40310

ord-86101b2e7f9945179d50d853ef03d403

반응 방정식

CI
methyl iodide
[H-].[K+]
potassium hydride
CC1CCCCC1=O
2-methylcyclohexanone
CCB(CC)CC
Triethylborane
CC1(C)CCCCC1=O
title compound
CC1(C)CCCCC1=O
2,2-dimethyl-cyclohexanone

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe mixture is stirred for 16 hours at room temperature
  2. 2
    workup.WAITis continued for another 8 hours
  3. 3
    기타the reaction is then quenched with saturated aqueous ammonium chloride solution
  4. 4
    추출twice extracted with diethyl ether
  5. 5
    건조The combined organic phases are dried over sodium sulphate
  6. 6
    농축concentrated to dryness in a vacuum

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07727979B2uspto-grants-2010_06