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

HRID 1916043노트

반응식

HRID 1916043 반응식
[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]

참가 물질

4

반응물 2

HCID 6371PhosgeneHCID 922497-Amino-4-methylcoumarin

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-1ea8e4a90d66403db1059313f7f9be6e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618096B2

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