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HRID2301504

反应详情

EQUATION

反应方程式

HRID 2301504 的结构方程式

REACTANTS

反应物

3
结构：CCO
HCID702

Ethanol

C2H6O

结构：C[Si](C)(C)Cl
HCID6397

Chlorotrimethylsilane

C3H9ClSi

结构：CNS(=O)(=O)c1c(Cl)ccc([N+](=O)[O-])c1C(C)=O
HCID18373542

未命名化合物

PRODUCTS

生成物

1
结构：CNS(=O)(=O)c1c(Cl)ccc([N+](=O)[O-])c1O
HCID18373432

未命名化合物

收率 100%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：O=S(=O)(O)O
催化剂HCID1118

Sulfuric acid

H2O4S

PROCEDURE

实验过程

A solution of N-methyl-2-acetyl-6-chloro-3-nitrobenzenesulfonamide (170 mg, 0.55 mmol), 0.5 mL of chlorotrimethylsilane and 3 drops of fuming sulfuric acid in ethanol was heated to reflux for 20 hours. The solvent was evaporated. The residue was diluted with ethyl acetate and washed with water. The organic layer was then dried (Na2SO4) and concentrated to give the desired product (160 mg, >100%). EI-MS (m/z) 265.2, 267.2 (M−).

WORKUP

后处理

  1. temperatureto reflux for 20 hours
  2. customThe solvent was evaporated
  3. additionThe residue was diluted with ethyl acetate
  4. washwashed with water
  5. dry with materialThe organic layer was then dried (Na2SO4)
  6. concentrationconcentrated