반응 #75377

반응 방정식

3-sulphamoyl-4-phenoxy-5-[β-aminoethyl]-benzoic acid

acetonylacetone

aluminium

→

3-Sulphamoyl-4-phenoxy-5-[β-(2,5-dimethyl-1-pyrrolyl)-ethyl]-benzoic acid

용매

hexamethylphosphoric acid triamide

반응 조건

후처리

1. 1
   온도is warmed at 100° for 30 minutes under N2 in an apparatus which
2. 2
   추출extracting with ethyl acetate
3. 3
   세척washing the
4. 4
   추출extract with water
5. 5
   기타drying
6. 6
   여과filtering
7. 7
   기타evaporating the filtrate
8. 8
   기타The crude product is recrystallised from chloroform/cyclohexane with the addition of active charcoal
9. 9
   기타gives pale orange-coloured

실험 절차

A mixture of 3-sulphamoyl-4-phenoxy-5-[β-aminoethyl]-benzoic acid (5.0 g=1.35 mmols; see Example 3 for the preparation), acetonylacetone (1.85 g, approximately 16.2 mmols) and hexamethylphosphoric acid triamide (Hexametapol; 25 ml) is warmed at 100° for 30 minutes under N2 in an apparatus which has been protected against incident light by covering it with aluminium foil, and the reaction solution is worked up as follows, with strict exclusion of light throughout: pouring into ice-water (50 ml) and extracting with ethyl acetate, washing the extract with water, drying and filtering and evaporating the filtrate. The crude product is recrystallised from chloroform/cyclohexane with the addition of active charcoal and gives pale orange-coloured, light-sensitive crystals, melting point>210° (decomposition).

출처