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Dimethyl Sulfate → 1-(4-methoxyphenyl)-4-{4-[3-(methylthio)4H-1,2,4-triazol-4-yl]phenyl}piperazine

HRID 1154732
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HRID 1154732 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([N:21]4[CH:25]=[N:24][N:23]=[C:22]4[SH:26])=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[OH-].[Na+].S(OC)(O[CH3:33])(=O)=O>CO>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:10][CH2:11][N:12]([C:15]3[CH:20]=[CH:19][C:18]([N:21]4[CH:25]=[N:24][N:23]=[C:22]4[S:26][CH3:33])=[CH:17][CH:16]=3)[CH2:13][CH2:14]2)=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 1784919634-{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}-4H-1,2,4-triazole-3-thiol

생성물 1

HCID 128770271-(4-methoxyphenyl)-4-{4-[3-(methylthio)4H-1,2,4-triazol-4-yl]phenyl}piperazine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 9 parts of 4-{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}-4H-1,2,4-triazole-3-thiol, 2 parts of sodium hydroxide and 160 parts of methanol is stirred and warmed till all solid enters solution. Then there are added 3.3 parts of dimethyl sulfate and stirring is continued for 3 hours at room temperature. The reaction mixture is poured onto water. The precipitated product is filtered off and crystallized from 1-butanol, yielding 5.3 parts of 1-(4-methoxyphenyl)-4-{4-[3-(methylthio)-4H-1,2,4-triazol-4-yl]phenyl}piperazine; mp. 180° C.

후처리

  1. temperaturewarmed till all solid
  2. stirringstirring
  3. additionThe reaction mixture is poured onto water
  4. filtrationThe precipitated product is filtered off
  5. customcrystallized from 1-butanol

출처 및 근거

ORD 기록
ord-f653bfc0428c4bf8a9c2723a1349db39
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04490530

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