تفاعل #62548

ord-91b37a5954d74ff795689c1a0561d58a

معادلة التفاعل

COC(=O)CCl
Methyl chloroacetate
CN1CCNCC1
N-methylpiperazine
COC(=O)CN1CCN(C)CC1
2-(4-methyl-1-piperazinyl)acetic acid, methyl ester
المردود 95.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe reaction mixture was filtered
  2. 2
    أخرىthe solvent was removed under vacuum
  3. 3
    workup.DISSOLUTIONThe resulting oil was dissolved in methylene chloride-methanol (9:1)
  4. 4
    أخرىpurified by flash chromatography (silica)

الإجراء التجريبي

Methyl chloroacetate (8.8 ml., 0.10 mole) was added to a solution of N-methylpiperazine (24.4. ml., 0.22 mole) in ethyl acetate (140 ml.) and the mixture was stirred for 17 hours. The reaction mixture was filtered and the solvent was removed under vacuum. The resulting oil was dissolved in methylene chloride-methanol (9:1) and purified by flash chromatography (silica) to give 2-(4-methyl-1-piperazinyl)acetic acid, methyl ester as an oil (16.3 g, 95%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04761415uspto-grants-1988_08