تفاعل #50023

ord-597dbf67453e44ccb9afcd1128c217bb

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITAfter 16 hours at room temperature
  2. 2
    درجة الحرارةanother 4 hours at reflux
  3. 3
    درجة الحرارةheating
  4. 4
    درجة الحرارةat reflux
  5. 5
    workup.WAITcontinued for another 24 hr
  6. 6
    تركيزThe reaction mixture was then concentrated
  7. 7
    workup.WAITthe resultant oil was placed under high vacuum for several days

الإجراء التجريبي

To a solution of L-Proline (115 g,1 mol) in methanol (1.2 L) at 0° C. was added sulfuryl chloride (45 mL, 0.55 mol) slowly during ~15-20 min, then the reaction mixture stirred overnight at room temperature. After 16 hours at room temperature and another 4 hours at reflux, trimethyl orthoformate (120 mL, 1.1 mol) was added and heating at reflux continued for another 24 hr. The reaction mixture was then concentrated and the resultant oil was placed under high vacuum for several days to afford the product as a clear oil (205 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424444uspto-grants-1995_06