반응 #318920

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Phosgene

methyl 2-(aminosulfonyl)-4-ethoxybenzoate

n-butyl isocyanate

→

methyl 4-ethoxy-2-(isocyanatosulfonyl)benzoate

수율 98.4%

용매

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후처리

1. 1
   온도at reflux for 10 minutes
2. 2
   기타stayed at 133° C. or above
3. 3
   기타When consumption of phosgene
4. 4
   여과filtered under nitrogen
5. 5
   기타Rotary evaporation

실험 절차

A solution of methyl 2-(aminosulfonyl)-4-ethoxybenzoate (7.56 g/ 29.2 mmol), n-butyl isocyanate (3.29 mL, 29.2 mmol), and 1,4-diaza[2,2,2]bicyclooctane (0.13 g. 1.2 mmol) in mixed xylenes was heated at reflux for 10 minutes. Phosgene was then added at such a rate that the internal temperature stayed at 133° C. or above. When consumption of phosgene ceased, the solution was cooled to room temperature and then filtered under nitrogen. Rotary evaporation gave methyl 4-ethoxy-2-(isocyanatosulfonyl)benzoate as a cloudy yellow oil (8.2 g). This was used immediately without further purification or characterization.

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