Methane → HCID 86741874、化合物

HRID 247211ノート

反応式

HRID 247211 の反応式
O=[C:2](Cl)[O:3][C:4](Cl)(Cl)Cl.[C:9]([S:12][CH2:13][C@@H:14]([C:16]([OH:18])=[O:17])[NH2:15])(=[O:11])[CH3:10].C>O1CCOCC1>[N-:15]=[C:4]=[O:3].[CH3:2][O:17][C:16](=[O:18])[C@H:14]([CH2:13][S:12][C:9](=[O:11])[CH3:10])[NH2:15]

参加物

5

反応物 3

HCID 297MethaneHCID 10426DiphosgeneHCID 10130120S-Acetyl-Cysteine

生成物 1

HCID 86741874HCID 86741874、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 the methyl ester of S-acetylcysteine 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 S-acetylcysteine methyl 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 filtrate is fractionally distilled

出典と根拠

ORDレコード
ord-538284040cca481b9c36f1ead1da20b2
出典データセット
uspto-grants-1987_11
特許番号
US04705864

反応ノート

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