海萝胶 → N-(2,5-difluorophenyl)benzenesulfonamide

HRID 4234

反应方程式

HRID 4234 反应方程式
[F:1][C:2]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:3]=1[NH2:4].N1C=CC=CC=1.[C:16]1([S:22](Cl)(=[O:24])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.Cl>O>[F:1][C:2]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:3]=1[NH:4][S:22]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)(=[O:24])=[O:23]

参与物

6

反应物 4

HCID 313海萝胶HCID 1049吡啶HCID 7369苯磺酰氯HCID 677752,5-二氟苯胺

产物 1

HCID 8500589N-(2,5-difluorophenyl)benzenesulfonamide

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
40 °C

实验过程

0.194 mole (25 g) of 2,5-difluoroaniline is added to 125 ml of pyridine. 0.2 mole (25.5 ml) of benzenesulphonyl chloride is added, while the temperature is between 35° C. and 45° C. The temperature is maintained at 40° C. for 1 hour after the addition is completed, and then the reaction mixture is poured onto 1 kg of ice and water to which 100 ml of concentrated hydrochloric acid have been added. The expected product precipitates. After filtration and washing, it is treated with a normal sodium hydroxide solution in order to remove insoluble material. The soda-containing filtrate is neutralized with concentrated hydrochloric acid. The expected product, which has precipitated, is filtered off, washed to neutrality and recrystallized from acetic acid. It melts at 115° C.

后处理

  1. customis between 35° C. and 45° C
  2. additionafter the addition
  3. additionhave been added
  4. customThe expected product precipitates
  5. filtrationAfter filtration
  6. washwashing
  7. additionit is treated with a normal sodium hydroxide solution in order
  8. customto remove insoluble material
  9. customThe expected product, which has precipitated
  10. filtrationis filtered off
  11. washwashed to neutrality
  12. customrecrystallized from acetic acid

来源与证据

ORD记录
ord-3dbdfcae709944628a41bf0158fca242
来源数据集
uspto-grants-1988_02
专利号
US04725283

关联笔记

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