반응 #472328

반응 방정식

2,3-dihydro-1,3-benzothiazole

2-aminobenzenethiol

formalin

3-cyano-4-methoxy-5-trifluoromethoxybenzoyl chloride

→

3-(3-cyano-4-methoxy-5-trifluoromethoxybenzoyl)-2,3-dihydro-1,3-benzothiazole

용매

chloroform

triethylamine

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure and water
2. 2
   workup.ADDITIONwas added
3. 3
   추출the mixture was extracted with ethyl acetate
4. 4
   세척The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
7. 7
   기타the obtained residue was used for the synthesis of (j)

실험 절차

2,3-dihydro-1,3-benzothiazole synthesized from 2-aminobenzenethiol (359 mg) and 37% formalin (0.24 mL) in the same manner as in Example 1 was dissolved in chloroform (10 mL), and triethylamine (0.80 mL) and 3-cyano-4-methoxy-5-trifluoromethoxybenzoyl chloride were added to the solution, and then the mixture was stirred at room temperature for 17 hours. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was used for the synthesis of (j).

출처