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Thiosemicarbazide Hydrochloride → HCID 178491699、化合物

HRID 1088536
ノート
印刷プレビュー

反応式

HRID 1088536 の反応式
C(O[C:4]1[CH2:8][CH:7]([S:9][CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[CH2:6][N:5]=1)C.Cl.[NH2:20][NH:21][C:22]([NH2:24])=[S:23]>C(O)C>[CH3:18][O:17][C:14]1[CH:15]=[CH:16][C:11]([CH2:10][S:9][CH:7]2[CH2:6][NH:5][C:4](=[N:20][NH:21][C:22]([NH2:24])=[S:23])[CH2:8]2)=[CH:12][CH:13]=1
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 2

HCID 3037943Thiosemicarbazide HydrochlorideHCID 104680652-Ethoxy-4-p-methoxybenzylthio-1-pyroline

生成物 1

HCID 178491699HCID 178491699、化合物収率 21.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-ethoxy-4-p-methoxybenzylthio-1-pyrroline (900 mg) and thiosemicarbazide hydrochloride (433 mg) in ethanol (30 ml) was refluxed under heating for 1.5 hours. The reaction solution was evaporated to dryness under reduced pressure, then the residue was distributed between ethyl acetate and 5% aqueous solution of sodium hydroxide and the organic phase was dried over Na2SO4 before the solvent was distilled off under reduced pressure. The resultant residue was passed through a column packed with 25 g of silica gel and eluted with ethyl acetate and thus 230 mg of the objective compound was obtained as colorless foam.

後処理

  1. temperatureunder heating for 1.5 hours
  2. customThe reaction solution was evaporated to dryness under reduced pressure
  3. dry with materialthe organic phase was dried over Na2SO4 before the solvent
  4. distillationwas distilled off under reduced pressure
  5. washeluted with ethyl acetate

出典と根拠

ORDレコード
ord-94973597c9e0477d9a173b09b1614913
出典データセット
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04962202

反応ノート

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