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Ethanol → HCID 178470470、化合物

HRID 2052248
ノート
印刷プレビュー

反応式

HRID 2052248 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([CH2:7][N:8]=[C:9]=[S:10])=[CH:5][CH:4]=1.[C:13]([NH:18][NH2:19])(=O)[C:14]([OH:16])=[O:15].[CH2:20](O)[CH3:21]>>[CH2:20]([O:16][C:14]([C:13]1[N:8]([CH2:7][C:6]2[CH:11]=[CH:12][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[C:9]([SH:10])=[N:19][N:18]=1)=[O:15])[CH3:21]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 702EthanolHCID 1231974-Methoxybenzyl isothiocyanateHCID 222877Hydrazino(oxo)acetic acid

生成物 1

HCID 178470470HCID 178470470、化合物

実験手順

A solution of p-methoxybenzyl isothiocyanate (8.95 g.) and the ethyl ester of oxalic acid monohydrazide (6.8 g.) in ethanol (50 ml.) was refluxed for a period of approximately 16 hours (overnight). The hot solution was then filtered, the filtrate evaporated in vacuo and the resulting oil triturated with dry diethyl ester. The solid product so obtained, viz., 3-ethoxycarbonyl-4-(p-methoxybenzyl)-1,2,4-triazole-5-thiol (yield, 7.2 g.) was then recrystallized from ethanol-water to yield 4.0 g. of pure material. The analytical sample melted at 142°-144° C. after a further recrystallization from ethyl acetate/petroleum ether (b.p. 60°-80° C.).

後処理

  • filtrationThe hot solution was then filtered
  • customthe filtrate evaporated in vacuo
  • customthe resulting oil triturated with dry diethyl ester
  • customThe solid product so obtained
  • custom, 3-ethoxycarbonyl-4-(p-methoxybenzyl)-1,2,4-triazole-5-thiol (yield, 7.2 g.) was then recrystallized from ethanol-water
  • customto yield 4.0 g
  • customThe analytical sample melted at 142°-144° C. after a further recrystallization from ethyl acetate/petroleum ether (b.p. 60°-80° C.)
  • 出典と根拠

    ORDレコード
    ord-3feb0b11833f4aabb62e3b7150fdf252
    出典データセット
    uspto-grants-1980_01
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04183925

    反応ノート

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