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2-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonate → 1-[2-(2,4-Dichlorophenyl)-2-hydroxy-3-(thiazol-2-ylthio)propyl]-1,2,4-triazole

HRID 2118492
ノート
印刷プレビュー

反応式

HRID 2118492 の反応式
CS(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[C:14]1([CH2:17][N:18]2[CH:22]=[N:21][CH:20]=[N:19]2)[CH2:16][O:15]1.[SH:23][C:24]1[S:25][CH:26]=[CH:27][N:28]=1>C(O)(=O)C>[Cl:6][C:7]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:8]=1[C:14]([OH:15])([CH2:16][S:23][C:24]1[S:25][CH:26]=[CH:27][N:28]=1)[CH2:17][N:18]1[CH:22]=[N:21][CH:20]=[N:19]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 867396002-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonateHCID 178527881HCID 178527881、化合物

生成物 1

HCID 201939471-[2-(2,4-Dichlorophenyl)-2-hydroxy-3-(thiazol-2-ylthio)propyl]-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

2-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane, methanesulphonate salt, (6 g, 0.0164 m) and 2-mercaptothiazole (6 g, 0.05 m) were heated in glacial acetic acid (200 ml) under refluxed for 4 hours. The solvent was then evaporated and the residue was basified with dilute sodium hydroxide solution and extracted with methylene chloride. The extract was washed once with dilute sodium hydroxide solution, dried (MgSO4) and evaporated to give a pale brown glass (5.4 g) which was chromatographed on silica, eluting with ethyl acetate:ether:methanol:diethylamine 25:75:2:2, to give, after one recrystallization from isopropanol, the title compound 2 g, (32%); m.p. 110°-111° C.

後処理

  1. temperatureunder refluxed for 4 hours
  2. customThe solvent was then evaporated
  3. extractionextracted with methylene chloride
  4. washThe extract was washed once with dilute sodium hydroxide solution
  5. dry with materialdried (MgSO4)
  6. customevaporated

出典と根拠

ORDレコード
ord-6881f6dad1104d698232e5bf2ccb8b7f
出典データセット
uspto-grants-1987_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04678789

反応ノート

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