Methane → Asparagine methyl ester isocyanate
반응식
[O:1]=[C:2](Cl)[O:3][C:4](Cl)(Cl)Cl.[NH2:9][C@H:10](C(O)=O)[CH2:11][C:12](=[O:14])[NH2:13].C>O1CCOCC1>[N-:13]=[C:12]=[O:14].[CH3:4][O:3][C:2](=[O:1])[C@H:10]([CH2:11][C:12](=[O:14])[NH2:13])[NH2:9]참가 물질
5
실험 절차
0.35 mol diphosgene is added dropwise over 1 hour to a mixture of 0.28 mol of the methyl ester of asparagine 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 re-dissolved 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 filtrate is fractionally distilled to give asparagine methyl 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 re-dissolved 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 filtrate is fractionally distilled
출처 및 근거
- ORD 기록
- ord-44921723b7b74232a6e687ac4c5d88c4
- 출처 데이터셋
- uspto-grants-1987_11
- 특허 번호
- US04705864
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