تفاعل #69129

ord-ec34a7563eb44511b2b3a924494ca26f

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added dropwise
  2. 2
    غسيلThe crude mixture was washed with 1M HCl, water
  3. 3
    تجفيفThe organic extracts were dried over magnesium sulfate
  4. 4
    ترشيحfiltered
  5. 5
    تركيزconcentrated in vacuo

الإجراء التجريبي

Cis-(R)-tert-butyl 1-(4-hydroxycyclohexyl)ethylcarbamate (575 mg, 2.363 mmol) was dissolved in dichloromethane (10 mL) and cooled to 0° C. under nitrogen. Triethylamine (478.2 mg, 658.7 μL, 4.726 mmol) followed by methanesulfonylchloride (284.2 mg, 192.0 μL, 2.481 mmol) were added dropwise. The reaction mixture was stirred at room temperature for 30 minutes. The crude mixture was washed with 1M HCl, water and a saturated aqueous solution of sodium bicarbonate. The organic extracts were dried over magnesium sulfate, filtered and concentrated in vacuo to give the compound as a white solid (706 mg, 93% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08530489B2uspto-grants-2013_09