Methane → Glycine isopropyl ester isocyanate
반응식
O=C(Cl)[O:3][C:4](Cl)(Cl)Cl.[CH:9]([O:12][C:13](=[O:16])[CH2:14][NH2:15])([CH3:11])[CH3:10].C>O1CCOCC1>[N-:15]=[C:4]=[O:3].[CH:9]([O:12][C:13](=[O:16])[CH2:14][NH2:15])([CH3:11])[CH3:10]참가 물질
5
실험 절차
0.35 mol diphosgene is added dropwise over 1 hour to a mixture of 0.28 mol of glycine isopropyl ester and 0.4 g activated charcoal in 400 mL dioxane under N2. The reaction mixture is then heated and stirred at reflux for 21/2 hours. The reaction mixture is then cooled, filtered, and concentrated to dryness by rotary evaporator, keeping exposure to moisture to a minimum. The crude product is redissolved in 100 mL THF, and the pH of the solution is adjusted to 5.5-6.0 by addition of pyridine. The product mixture is again filtered, and the product is purified by fractional distillation to give glycine isopropyl ester isocyanate.
후처리
- temperatureThe reaction mixture is then heated
- temperatureat reflux for 21/2 hours
- temperatureThe reaction mixture is then cooled
- filtrationfiltered
- concentrationconcentrated to dryness by rotary evaporator
- dissolutionThe crude product is redissolved in 100 mL THF
- additionthe pH of the solution is adjusted to 5.5-6.0 by addition of pyridine
- filtrationThe product mixture is again filtered
- distillationthe product is purified by fractional distillation
출처 및 근거
- ORD 기록
- ord-85a093ff85c54253a6d03ec059d67ee6
- 출처 데이터셋
- uspto-grants-1990_12
- 특허 번호
- US04977272
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