Hydrochloric Acid → 5-Chloro-3-methyl-6-(pyrrol-1-yl)-benzofuran

HRID 637695노트

반응식

HRID 637695 반응식
Cl.[NH2:2][C:3]1[C:12]([Cl:13])=[CH:11][C:6]2[C:7]([CH3:10])=[CH:8][O:9][C:5]=2[CH:4]=1.CO[CH:16]1[CH2:20][CH2:19][CH:18](OC)O1>O1CCOCC1>[Cl:13][C:12]1[C:3]([N:2]2[CH:16]=[CH:20][CH:19]=[CH:18]2)=[CH:4][C:5]2[O:9][CH:8]=[C:7]([CH3:10])[C:6]=2[CH:11]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 790982,5-DimethoxytetrahydrofuranHCID 202556476-Amino-5-chloro-3-methylbenzofuran

생성물 1

HCID 202556465-Chloro-3-methyl-6-(pyrrol-1-yl)-benzofuran

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

7 ml of 5N hydrochloric acid are added to a mixture of 9.1 g (50 mmole) of 6-amino-5-chloro-3-methylbenzofuran, 10 ml (78 mmole) of 2,5-dimethoxytetrahydrofuran and 200 ml of dioxane and the whole is stirred at room temperature for 16 hours. The whole is subsequently concentrated by evaporation in vacuo and the residue is chromatographed over silica gel with petroleum ether/methylene chloride. Crystallisation of the resulting product from petroleum ether yields 5-chloro-3-methyl-6-(pyrrol-1-yl)-benzofuran having a melting point of 49°-52°.

후처리

  1. concentrationThe whole is subsequently concentrated by evaporation in vacuo
  2. customthe residue is chromatographed over silica gel with petroleum ether/methylene chloride
  3. customCrystallisation of the resulting product from petroleum ether

출처 및 근거

ORD 기록
ord-e54f226f218f4830919c9ad19dad9aec
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558043

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