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

HRID 637695ノート

反応式

HRID 637695 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-e54f226f218f4830919c9ad19dad9aec
出典データセット
uspto-grants-1985_12
特許番号
US04558043

反応ノート

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