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

HRID 2286545
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HRID 2286545 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-80f2e9bdbb574d739878a65f4819776f
출처 데이터셋
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04267179

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