Methane → Glycine isopropyl ester isocyanate
反応式
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]参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-85a093ff85c54253a6d03ec059d67ee6
- 出典データセット
- uspto-grants-1990_12
- 特許番号
- US04977272
反応ノート
読み込み中…