Methanol → HCID 12877063, 화합물

HRID 1154733노트

반응식

HRID 1154733 반응식
CO.[CH3:3][C:4]1[N:8]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=2)[N:7]=[C:6]([SH:18])[N:5]=1.[OH-].[Na+].S(OC)(O[CH3:25])(=O)=O>O>[CH3:3][C:4]1[N:8]([C:9]2[CH:10]=[CH:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=2)[N:7]=[C:6]([S:18][CH3:25])[N:5]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 178433555HCID 178433555, 화합물

생성물 1

HCID 12877063HCID 12877063, 화합물수율 66%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 80 parts of methanol are added 4.7 parts of 5-methyl-1-(4-nitrophenyl)-1H-1,2,4-triazole-3-thiol and 1.2 parts of sodium hydroxide and the whole is stirred till all solid enters solution. Then there are added 2.66 parts of dimethyl sulfate and stirring is continued for 1 hour at room temperature. 100 Parts of water are added. The precipitated product is filtered off, washed with water, dried, and crystallized from 2,2'-oxybispropane, yielding 3.3 parts (66%) of 5-methyl-3-(methylthio)-1-(4-nitrophenyl)-1H-1,2,4-triazole; mp. 121°-125° C.

후처리

  1. stirringstirring
  2. filtrationThe precipitated product is filtered off
  3. washwashed with water
  4. customdried
  5. customcrystallized from 2,2'-oxybispropane

출처 및 근거

ORD 기록
ord-2262f884be054effb095e8cb4bff6eed
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04490530

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