Phosgene → 7-isocyanato-4-methyl-2H-chromen-2-one

HRID 1916043ノート

反応式

HRID 1916043 の反応式
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:13])=[CH:7][C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1.[C:14](Cl)(Cl)=[O:15]>C1(C)C=CC=CC=1>[N:1]([C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:13])=[CH:7][C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1)=[C:14]=[O:15]

参加物

4

反応物 2

HCID 6371PhosgeneHCID 922497-Amino-4-methylcoumarin

生成物 1

HCID 583781007-isocyanato-4-methyl-2H-chromen-2-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A round bottom flask was charged with 7-amino-4-methyl-coumarin (50 mg, 0.285 mmol) under argon and treated with a 20% phosgene in toluene solution (2 ml) under. The reaction mixture was heated at reflux for 15 hrs under argon during which time a white solid precipitated out of solution. After cooling, the excess phosgene was removed by bubbling argon gas through from the solution for 10 minutes. The reaction mixture was then evaporated to afford the product as white solid, which was used directly in the next step. Yield: 50 mg (87%).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 15 hrs under argon during which time a white solid
  3. customprecipitated out of solution
  4. temperatureAfter cooling
  5. customthe excess phosgene was removed
  6. customby bubbling argon gas through from the solution for 10 minutes
  7. customThe reaction mixture was then evaporated

出典と根拠

ORDレコード
ord-1ea8e4a90d66403db1059313f7f9be6e
出典データセット
uspto-grants-2013_12
特許番号
US08618096B2

反応ノート

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