Acetic Acid → 2-(3-Methoxy-2-nitrophenyl)-4H-chromen-4-one

HRID 260086노트

반응식

HRID 260086 반응식
C(O)(=O)C.S(=O)(=O)(O)O.O[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[C:17](=[O:32])[CH2:18][C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([O:27][CH3:28])[C:22]=1[N+:29]([O-:31])=[O:30])=[O:20]>O>[CH3:28][O:27][C:23]1[C:22]([N+:29]([O-:31])=[O:30])=[C:21]([C:19]2[O:20][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[C:17](=[O:32])[CH:18]=2)[CH:26]=[CH:25][CH:24]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 224024981-(2-Hydroxyphenyl)-3-(3-methoxy-2-nitrophenyl)propane-1,3-dione

생성물 1

HCID 224024972-(3-Methoxy-2-nitrophenyl)-4H-chromen-4-one수율 70.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of glacial acetic acid (15 mL), concentrated sulfuric acid (180 mL), and 1-(2-hydroxy-phenyl)-3-(3-methoxy-2-nitrophenyl)propane -1,3 -dione (770 mg, 2.43 mmol) is heated at reflux for 2.5 hours. The hot solution is poured onto crushed ice and H2O (200 mL), stirring vigorously for 30 minutes. The solution is cooled in a refrigerator. The resulting solid is filtered and washed with H2O to yield 2-(3-methoxy-2-nitrophenyl)-4-oxo-4H-[1]benzopyran (510 mg, 70%) as a brown solid.

후처리

  1. temperatureat reflux for 2.5 hours
  2. additionThe hot solution is poured
  3. temperatureThe solution is cooled in a refrigerator
  4. filtrationThe resulting solid is filtered
  5. washwashed with H2O

출처 및 근거

ORD 기록
ord-9639366cc73c4670aed65e75b942fc59
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05525625

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