哌嗪二盐酸盐 → 4-派嗪-1-甲基苯甲酸甲酯

HRID 2290450

反应方程式

HRID 2290450 反应方程式
O.O.O.O.O.O.[NH:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.Cl.Cl.N1CCNCC1.Br[CH2:22][C:23]1[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=1>CO>[N:7]1([CH2:22][C:23]2[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=2)[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1

参与物

5

反应物 3

HCID 8893哌嗪二盐酸盐HCID 120181哌嗪(六水)HCID 2566874-溴甲基苯甲酸甲酯

产物 1

HCID 70186274-派嗪-1-甲基苯甲酸甲酯收率 64%

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

A mixtue of 38 g. (0.2 mole) piperazine hexahydrate, 28 g. (0.2 mole) piperazine dihydrochloride and 150 ml. methanol is mixed, while stirring at ambient temperature, with 45 g. (0.2 mole) methyl 4-bromomethylbenzoate. The reaction mixture is left to stand for 2 days and suction filtered from the precipitate. The clear solution is evaporated and the residue is recrystallised from ethanol to give 39 g. (64%) of the desired compound as a monohydrochloride; m.p. 226°-227° C.

后处理

  1. waitThe reaction mixture is left
  2. filtrationsuction filtered from the precipitate
  3. customThe clear solution is evaporated
  4. customthe residue is recrystallised from ethanol
  5. customto give 39 g

来源与证据

ORD记录
ord-c2a1209efed14541a56982e6500c44bc
来源数据集
uspto-grants-1986_10
专利号
US04616086

关联笔记

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