تفاعل #8923

ord-de60f6eb45574755aa855b738efb7294

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    أخرىA 100 mL round bottom flask equipped with magnetic stir bar
  2. 2
    أخرىAfter 1 hour reaction
  3. 3
    تركيزwas concentrated in vacuo
  4. 4
    غسيلthe organic phase was washed with saturated aqueous bicarb
  5. 5
    تجفيف, brine, dried
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

A 100 mL round bottom flask equipped with magnetic stir bar was charged with 0.42 mL (1.05 eq) N-methyl-piperazine, 1 mL NEt3 and 20 mL CH2Cl2. The solution was cooled to 0° C. and 1.0 g of benzyl 3-chlorosulfonyl-2(R)-methylpropionate from Example 3 in 5 mL CH2Cl2 was added. After 1 hour reaction was concentrated in vacuo. The residue was partioned between EA/H2O and the organic phase was washed with saturated aqueous bicarb., brine, dried, and concentrated in vacuo to yield benzyl 3-[(4-methylpiperizin-1-yl)sulfonyl]-2(R)-methylpropionate which was used without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091219B2uspto-grants-2006_08