反応 #985261

ord-5604215748e24f859d16b9a30f4d0eab

反応方程式

O=C(Cl)c1ccc([N+](=O)[O-])cc1
4-nitrobenzoyl chloride
Nc1ccccc1S
2-aminothiophenol
O=[N+]([O-])c1ccc(-c2nc3ccccc3s2)cc1
product
収率 73.2%
O=[N+]([O-])c1ccc(-c2nc3ccccc3s2)cc1
2-(4-Nitrophenyl)benzothiazole
収率 73.2%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction was quenched with water (20 mL)
  2. 2
    その他The aqueous layer was separated
  3. 3
    抽出extracted with ethyl acetate (3×10 ml)
  4. 4
    その他The combined organic layers were dried
  5. 5
    その他evaporated
  6. 6
    その他The crude product was purified
  7. 7
    その他with flush column, (hexane:ethyl acetate=85:15)

実験手順

A solution of 4-nitrobenzoyl chloride (1.49 g, 8.0 mmol) in benzene anhydrous, 10 mL) was added dropwise to 2-aminothiophenol (1.0 g, 8.0 mmol in 10 ml of benzene) at room temperature. The reaction mixture was allowed to stir for 16 hr. The reaction was quenched with water (20 mL). The aqueous layer was separated and extracted with ethyl acetate (3×10 ml). The combined organic layers were dried and evaporated. The crude product was purified with flush column, (hexane:ethyl acetate=85:15) to give 1.5 g (73.2%) of product as light yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07351401B2uspto-grants-2008_04