تفاعل #1163395

ord-5510e451777049eca51dfd55023ae932

معادلة التفاعل

CN1CCNCC1
4-methylpiperazine
Cc1c(CO)nc2n1-c1ccccc1N(C)c1ccccc1-2
3,9-dimethyl-2-hydroxymethyl-9H-dibenzo[b,f]-imidazo[1,2-d] [1,4]diazepine
C1CCOC1.ClC(Cl)Cl
chloroform tetrahydrofuran
CS(=O)(=O)Cl
methanesulfonyl chloride
Cc1c(CN2CCN(C)CC2)nc2n1-c1ccccc1N(C)c1ccccc1-2
3,9-dimethyl-2-(4-methyl-1-piperazinyl)methyl-9H-dibenz[b,f]-imidazo[1,2-d][1,4]diazepine

المذيبات

ظروف التفاعل

درجة الحرارة
-20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONis added
  2. 2
    درجة الحرارةwarmed gradually to room temperature
  3. 3
    أخرىfollowed by the usal purification techniques

الإجراء التجريبي

A sampmle of 3,9-dimethyl-2-hydroxymethyl-9H-dibenzo[b,f]-imidazo[1,2-d] [1,4]diazepine is suspended in a chloroform/tetrahydrofuran mixture and treated with triethylamine. After cooling to -20° C. methanesulfonyl chloride is added with stirring at -20° C. The mixture is treated with 4-methylpiperazine and warmed gradually to room temperature. Work-up from an aqueous base followed by the usal purification techniques affords the product 3,9-dimethyl-2-(4-methyl-1-piperazinyl)methyl-9H-dibenz[b,f]-imidazo[1,2-d][1,4]diazepine as a yellow oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US03956297uspto-grants-1976_05