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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
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HRID 2118492 반응식
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
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참가 물질

4

반응물 2

HCID 867396002-(2,4-Dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonateHCID 178527881HCID 178527881, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6881f6dad1104d698232e5bf2ccb8b7f
출처 데이터셋
uspto-grants-1987_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04678789

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