تفاعل #8943

ord-23f9c4ecd6c3478fab0005d763040104

الكواشف

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المذيبات

ظروف التفاعل

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
    تركيزThe reaction was concentrated to half volume
  3. 3
    أخرىpartitioned between Et2O and H2O
  4. 4
    استخلاصextracted with 2×75 mL ethyl acetate
  5. 5
    أخرىThe combined organics were dried
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

A 100 mL round bottom flask equipped with magnetic stirring bar and N2 inlet was charged with 3.0 g benzyl 3-(4-benzylpiperizin-1-ylsulfonyl)-2(R)-methylpropionate, 1.2 g LiOH (4 eq.) in 20 mL 50% aqueous methanol. After 2 hours HPLC analysis showed no starting material. The reaction was concentrated to half volume and partitioned between Et2O and H2O. The aqueous layer was acidified to pH 5 and extracted with 2×75 mL ethyl acetate. The combined organics were dried, and concentrated in vacuo to yield 550 mg (25%) white solid.

المصدر

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