三乙胺 → 特拉唑嗪

HRID 619669

反应方程式

HRID 619669 反应方程式
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([N:16]2[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)[N:3]=1.C(N(CC)CC)C.[O:29]1[CH2:33][CH2:32][CH2:31][CH:30]1[C:34](Cl)=[O:35]>C(Cl)Cl>[CH3:13][O:12][C:9]1[CH:10]=[C:11]2[C:2]([NH2:1])=[N:3][C:4]([N:16]3[CH2:21][CH2:20][N:19]([C:34]([CH:30]4[O:29][CH2:33][CH2:32][CH2:31]4)=[O:35])[CH2:18][CH2:17]3)=[N:5][C:6]2=[CH:7][C:8]=1[O:14][CH3:15]

参与物

5

反应物 3

HCID 8471三乙胺HCID 551254四氢呋喃-2-甲酰氯HCID 6162672-哌嗪基-4-氨基-6,7-二甲氧基喹唑啉

产物 1

HCID 5401特拉唑嗪收率 154.9%

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

反应条件

温度
-5 °C

实验过程

37.6 g 4-amino-2-(1-piperazinyl)-6,7-dimethoxyquinazoline and 15.8 g triethylamine are suspended in 400 ml methylene chloride. The suspension is cooled to -5° C. This suspension is stirred while 21.0 g tetrahydrofuran-2-carboxylic acid chloride are added drop by drop. The suspension is continued to be stirred for two hours at 0° C., thereafter the solvent is distilled off under vacuum. 200 ml methanol and 200 ml acetone are added to the residue. The resulting suspension is kept under reflux for 0.5 hours while stirring. Thereafter, it is cooled to 0° C. The product is isolated by filtration. 78 g of moist terazosin base are obtained.

后处理

  1. additionare added drop by drop
  2. distillationthe solvent is distilled off under vacuum
  3. addition200 ml methanol and 200 ml acetone are added to the residue
  4. temperatureunder reflux for 0.5 hours
  5. stirringwhile stirring
  6. temperatureThereafter, it is cooled to 0° C
  7. customThe product is isolated by filtration

来源与证据

ORD记录
ord-30e79277aa3a428797898df30a3543a7
来源数据集
uspto-grants-1999_09
专利号
US05959108

关联笔记

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