تفاعل #40310

ord-86101b2e7f9945179d50d853ef03d403

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07727979B2uspto-grants-2010_06