碳酸钾 → Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-cyclopropylmethyl-4-oxo-1,4-dihydroquinoline-3-carboxylate

HRID 4562

反应方程式

HRID 4562 反应方程式
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1)[N:8]=[CH:7][C:6]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:5]2[OH:22].C(=O)([O-])[O-].[K+].[K+].[CH:29]1([CH2:32]Br)[CH2:31][CH2:30]1>CN(C)C=O>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:12]1[CH:16]=[CH:15][CH:14]=[CH:13]1)[N:8]([CH2:32][CH:29]1[CH2:31][CH2:30]1)[CH:7]=[C:6]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:5]2=[O:22]

参与物

5

反应物 3

HCID 11430碳酸钾HCID 81503溴甲基环丙烷HCID 178418515HCID 178418515，化合物

产物 1

HCID 13670064Ethyl 6-fluoro-7-(pyrrol-1-yl)-1-cyclopropylmethyl-4-oxo-1,4-dihydroquinoline-3-carboxylate收率 62.3%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
80 °C

实验过程

A mixture of 3.6 g (0.012 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-4-hydroxyquinoline-3-carboxylate and 4.15 g (0.03 mol) of potassium carbonate in 30 ml of dimethlformamide is heated for 30 minutes at 80° C. and left to cool, 8 g (0.06 mol) of cyclopropylmethyl bromide are added, the mixture is kept for 12 hours at 90° C. and left to cool, 80 ml of a water/ice mixture are added and the precipitate formed is filtered off, washed with water and recrystallized from ethanol to give 2.65 g of a solid melting at 125°-127° C.

后处理

  1. waitleft
  2. temperatureto cool
  3. waitleft
  4. temperatureto cool
  5. customthe precipitate formed
  6. filtrationis filtered off
  7. washwashed with water
  8. customrecrystallized from ethanol

来源与证据

ORD记录
ord-fd0d21daeb32407586c452e4c390cba8
来源数据集
uspto-grants-1988_02
专利号
US04727080

关联笔记

加载中…