Ammonium Hydroxide → Pyridazine, 5-methyl-3-[3-(trifluoromethyl)phenyl]-

HRID 1731717노트

반응식

HRID 1731717 반응식
Cl[C:2]1[N:3]=[N:4][C:5]([C:9]2[CH:10]=[C:11]([C:15]([F:18])([F:17])[F:16])[CH:12]=[CH:13][CH:14]=2)=[CH:6][C:7]=1[CH3:8].[NH4+].[OH-]>[Pd].CO>[CH3:8][C:7]1[CH:6]=[C:5]([C:9]2[CH:10]=[C:11]([C:15]([F:17])([F:16])[F:18])[CH:12]=[CH:13][CH:14]=2)[N:4]=[N:3][CH:2]=1

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 12449558HCID 12449558, 화합물

생성물 1

HCID 10657542Pyridazine, 5-methyl-3-[3-(trifluoromethyl)phenyl]-수율 78.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To 3-chloro-4-methyl-6-(α,α,α-trifluoro-m-tolyl)pyridazine(7 g) is added 10% palladium on carbon catalyst (0.7 g) and 300 mL of MeOH containing 30 mL of concentrated NH4OH. The mixture is shaken with H2 until the uptake of H2 ceases. The mixture is filtered to remove catalyst and concentrated in vacuo and then diluted with CH2Cl2 /H2O. The organic phase is washed with water and dried over MgSO4 to yield a solid which, on recrystallization from Et2O, gives 4.8 g (78%) of an off-white solid with a melting point of 114°-116° C.

후처리

  1. filtrationThe mixture is filtered
  2. customto remove catalyst
  3. concentrationconcentrated in vacuo
  4. additiondiluted with CH2Cl2 /H2O
  5. washThe organic phase is washed with water
  6. dry with materialdried over MgSO4
  7. customto yield a solid which
  8. customon recrystallization from Et2O

출처 및 근거

ORD 기록
ord-7780728892704690a50f601a94727f4b
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04623376

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