氨 → 4-甲氧基苯甲脒盐酸盐

HRID 1082081

反应方程式

HRID 1082081 反应方程式
[ClH:1].CO[C:4](=[NH:13])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][CH:6]=1.[NH3:14]>CO>[ClH:1].[CH3:12][O:11][C:8]1[CH:9]=[CH:10][C:5]([C:4]([NH2:13])=[NH:14])=[CH:6][CH:7]=1

参与物

4

反应物 2

HCID 222氨HCID 12463133Methyl 4-methoxybenzimidate hydrochloride

产物 1

HCID 123262194-甲氧基苯甲脒盐酸盐

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

35.9 g of 4-methoxybenzimidic acid methylester hydrochloride was dissolved in 300 ml of methanol. After saturation with ammonia gas under cooling in ice-water and stirring, the solution was stirred at room temperature for 15 hours. Then, methanol was evaporated in vacuo. Ethyl acetate was added to the residue. The precipitated crystals were filtered off and dried. Whereby 30.9 g of the desired substance was obtained as white crystals. Melting point is 220° to 221° C.

后处理

  1. stirringthe solution was stirred at room temperature for 15 hours
  2. customThen, methanol was evaporated in vacuo
  3. additionEthyl acetate was added to the residue
  4. filtrationThe precipitated crystals were filtered off
  5. customdried
  6. customWhereby 30.9 g of the desired substance was obtained as white crystals

来源与证据

ORD记录
ord-3445fba12d2a4bb7b66b3f276e7d1fab
来源数据集
uspto-grants-1996_12
专利号
US05589477

关联笔记

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