تفاعل #8942

ord-02bfd6ae3cc9411485ab357305a1bce2

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 stirring bar and N2 inlet
  2. 2
    تركيزthen concentrated in vacuo
  3. 3
    أخرىpartitioned between ethyl acetate and saturated sodium bicarbonate
  4. 4
    غسيلThe combined organics were washed with brine
  5. 5
    تجفيفdried over Na2SO4
  6. 6
    تركيزconcentrated in vacuo
  7. 7
    أخرىto yield 3.4 g crude product

الإجراء التجريبي

A 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet was charged with 2.5 g benzyl 3-chlorosulfonyl-2(R)-methylpropionate in 25 mL CH2Cl2. The solution was cooled to 0° C. and charged with 1.57 mL (1.0 eq.) 4-benzylpiperazine and 1.26 mL NEt3. The reaction was stirred for 1 hour then concentrated in vacuo and partitioned between ethyl acetate and saturated sodium bicarbonate. The combined organics were washed with brine, dried over Na2SO4, and concentrated in vacuo to yield 3.4 g crude product. Flash chromatography (80:20 ethyl acetate/hexane) yielded 3.0 g pure product.

المصدر

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