六水硝酸铽 → 6-fluoro-5-nitro-2(3H)-benzothiazolone

HRID 1761812

反应方程式

HRID 1761812 反应方程式
[F:1][C:2]1[CH:11]=[CH:10][C:5]2[NH:6][C:7](=[O:9])[S:8][C:4]=2[CH:3]=1.[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[F:1][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]2[NH:6][C:7](=[O:9])[S:8][C:4]=2[CH:3]=1

参与物

4

反应物 2

HCID 944六水硝酸铽HCID 446676-氟-2(3氢)苯噻唑酮

产物 1

HCID 139579556-fluoro-5-nitro-2(3H)-benzothiazolone收率 80.5%

试剂、催化剂与溶剂 1

HCID 1118四氧化硫溶剂

实验过程

A solution of 6-fluoro-2(3H)-benzothiazolone (47.58 g) in 100% sulfuric acid (760 ml) was cooled at 0° to 5° C., and 98% fuming nitric acid (d=1.52; 18.79 g) was dropwise added thereto, followed by stirring at the same temperatur for 60 minutes. The reaction mixture was poured into ice-water. The precipitated crystals were collected by filtration, washed with water and dried to give 6-fluoro-5-nitro-2(3H)-benzothiazolone (48.48 g) as pale brown crystals. m.p., 180°-182° C.

后处理

  1. filtrationThe precipitated crystals were collected by filtration
  2. washwashed with water
  3. customdried

来源与证据

ORD记录
ord-502f4cffdf864b9d845301fed04ec6f7
来源数据集
uspto-grants-1989_05
专利号
US04828605

关联笔记

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