Methane → HCID 86744409、化合物

HRID 1111030ノート

反応式

HRID 1111030 の反応式
O=C(Cl)[O:3][C:4](Cl)(Cl)Cl.[CH2:9]([O:12][C:13](=[O:17])[C@H:14]([CH3:16])[NH2:15])[CH:10]=[CH2:11].C>O1CCOCC1>[N-:15]=[C:4]=[O:3].[CH2:9]([O:12][C:13](=[O:17])[C@H:14]([CH3:16])[NH2:15])[CH:10]=[CH2:11]

参加物

5

反応物 3

HCID 297MethaneHCID 10426DiphosgeneHCID 10877480(S)-Allyl 2-aminopropanoate

生成物 1

HCID 86744409HCID 86744409、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 alanine allyl ester, prepared as described by H. Waldmann and H. Kunz in Liebigs Ann. Chem., 1983, 1712-1725, 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 alanine allyl ester isocyanate.

後処理

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

出典と根拠

ORDレコード
ord-0ddab3b52c4440e9a9531344759cf875
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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