Methane → HCID 86742132、化合物

HRID 1111006ノート

反応式

HRID 1111006 の反応式
O=C(Cl)[O:3][C:4](Cl)(Cl)Cl.[CH2:9]([O:12][C:13](=[O:16])[CH2:14][NH2:15])[CH2:10][CH3:11].C>O1CCOCC1>[N-:15]=[C:4]=[O:3].[CH2:9]([O:12][C:13](=[O:16])[CH2:14][NH2:15])[CH2:10][CH3:11]

参加物

5

反応物 3

HCID 297MethaneHCID 10426DiphosgeneHCID 2759255Propyl glycinate

生成物 1

HCID 86742132HCID 86742132、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.35 mol diphosgene is added dropwise over 1 hour to a mixture of 0.28 mol of glycine n-propyl 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 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 product is purified by fractional distillation to give glycine n-propyl ester isocyanate.

後処理

  1. temperatureThe reaction mixture is then heated
  2. temperatureat reflux for 21/2 hours
  3. temperatureThe reaction mixture is then cooled
  4. filtrationfiltered
  5. concentrationconcentrated to dryness by rotary evaporator
  6. dissolutionThe crude product is re-dissolved in 100 mL THF
  7. additionthe pH of the solution is adjusted to 5.5-6.0 by addition of pyridine
  8. filtrationThe product mixture is again filtered
  9. distillationthe product is purified by fractional distillation

出典と根拠

ORDレコード
ord-3578f660d5dd4a458fc6178ce1fae22e
出典データセット
uspto-grants-1990_12
特許番号
US04977272

反応ノート

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