تفاعل #53431

ord-f849e1c730c94e5db84ce2e7ae990baa

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    workup.STIRRINGthe mixture is stirred at 25° C. for 20 h
  2. 2
    تركيزAfter concentrating
  3. 3
    أخرىthe residue is partitioned between water and diethyl ether
  4. 4
    تجفيفthe ether phase is dried over sodium sulphate
  5. 5
    تركيزconcentrated
  6. 6
    أخرىThe product crystallizes out

الإجراء التجريبي

33.5 g, (0.3 mol of potassium tert-butoxide are initially introduced into 100 ml of anhydrous DMF at 0° C., and 51.6 g (0.25 mol) of the compound from Example XX in 250 ml of anhydrous DMF are added dropwise. The mixture is stirred at 0° C. for 30 min and 32.2 ml (0.3 mol) of cyclopentyl bromide in 150 ml of anhydrous DMF are added dropwise at 5-15° C. and the mixture is stirred at 25° C. for 20 h. After concentrating, the residue is partitioned between water and diethyl ether, and the ether phase is dried over sodium sulphate and concentrated. The product crystallizes out.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858622B2uspto-grants-2005_02