2,2-Diethoxytetrahydrofuran → 3,5-Dimethoxy-4-(pyrrol-1-yl)-benzoic acid methyl ester

HRID 462528

반응식

HRID 462528 반응식
C(O[C:4]1(OCC)[CH2:8][CH2:7][CH2:6]O1)C.[CH3:12][O:13][C:14](=[O:26])[C:15]1[CH:20]=[C:19]([O:21][CH3:22])[C:18]([NH2:23])=[C:17]([O:24][CH3:25])[CH:16]=1>C(O)(=O)C>[CH3:12][O:13][C:14](=[O:26])[C:15]1[CH:20]=[C:19]([O:21][CH3:22])[C:18]([N:23]2[CH:4]=[CH:8][CH:7]=[CH:6]2)=[C:17]([O:24][CH3:25])[CH:16]=1

참가 물질

4

반응물 2

HCID 3582902,2-DiethoxytetrahydrofuranHCID 123983034-Amino-3,5-dimethoxy-benzoic acid methyl ester

생성물 1

HCID 541987533,5-Dimethoxy-4-(pyrrol-1-yl)-benzoic acid methyl ester

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

온도
100 °C

실험 절차

A mixture of 9 g. of diethoxy-tetrahydrofuran and 5 ml. of glacial acetic acid was added dropwise at room temperature to a solution of 10.5 g. of 4-amino-3,5-dimethoxy-benzoic acid methyl ester in 50 ml. of glacial acetic acid with stirring. The mixture was stirred at 100° C. for an additional 30 minutes, cooled with ice, filtered under vacuum, dried and recrystallized from cyclohexane, whereby there was obtained 3,5-dimethoxy-4-(pyrrol-1-yl)-benzoic acid methyl ester having a melting point of 145°-146° C.

후처리

  1. additionA mixture of 9 g
  2. temperaturecooled with ice
  3. filtrationfiltered under vacuum
  4. customdried
  5. customrecrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-a9f3ebc8616d440ab6f0a516ce875729
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04515948

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