Methanol → R 61837

HRID 486471노트

반응식

HRID 486471 반응식
[CH3:1][O-:2].[Na+].[Na].CO.Cl[C:8]1[N:9]=[N:10][C:11]([N:14]2[CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[CH:21]=3)[CH2:16][CH2:15]2)=[CH:12][CH:13]=1>O>[CH3:1][O:2][C:8]1[N:9]=[N:10][C:11]([N:14]2[CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[CH:21]=3)[CH2:16][CH2:15]2)=[CH:12][CH:13]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 15124568HCID 15124568, 화합물

생성물 1

HCID 127504R 61837수율 50%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred sodium methoxide solution, previously prepared starting from 1.6 parts of sodium in 24 parts of methanol, were added 4 parts of 3-chloro-6-[4-(3-methylphenyl)-1-piperazinyl]pyridazine. The whole was stirred and refluxed for 40 hours. After cooling 25 parts of water were added. The product was filtered off, washed with water and dissolved in trichloromethane. The organic layer was dried, filtered and evaporated. The residue was crystallized from a mixture of 2-propanol and 2,2'-oxybispropane. The product was filtered off and dried, yielding 2 parts (50%) of 3-methoxy-6-[4-(3-methylphenyl)-1-piperazinyl]pyridazine; mp. 137.1° C. (compound 258).

후처리

  1. temperaturerefluxed for 40 hours
  2. additionwere added
  3. filtrationThe product was filtered off
  4. washwashed with water
  5. dissolutiondissolved in trichloromethane
  6. customThe organic layer was dried
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue was crystallized from a mixture of 2-propanol and 2,2'-oxybispropane
  10. filtrationThe product was filtered off
  11. customdried

출처 및 근거

ORD 기록
ord-b37c733004fb47d69e99b4a7c5fadde4
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292738

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