반응 #49182

반응 방정식

6-amino hexanoic acid

phthalic anhydride

triethyl amine

→

compound 41a

수율 93.8%

6-(1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-hexanoic acid

수율 93.8%

용매

toluene

반응 조건

후처리

1. 1
   온도The suspension was refluxed
2. 2
   기타When collection of water
3. 3
   온도the reaction was cooled
4. 4
   기타evaporated to dryness
5. 5
   workup.ADDITIONconc. hydrochloric acid (1.5 mL) was added
6. 6
   여과filtered
7. 7
   세척The precipitate was washed with water
8. 8
   건조dried over sodium sulfate

실험 절차

6-amino hexanoic acid (39a) (13.1 g, 100 mmol) and phthalic anhydride (40) (14.8 g, 100 mmol) were mixed in toluene (150 mL). To the suspension was added triethyl amine (13 mL). The suspension was refluxed using Dean-stark for 16 h. When collection of water ceased, the reaction was cooled and evaporated to dryness. The residue was suspended in water and conc. hydrochloric acid (1.5 mL) was added. The suspension was stirred for 30 mins and filtered. The precipitate was washed with water and dried over sodium sulfate to afford compound 41a (24.5 g, 93%) which was used as such for the next step.

출처