Triethylamine → 3,5-Diethyl-1-(2,4,6-trimethylphenyl)-1H-pyrazole

HRID 725276노트

반응식

HRID 725276 반응식
Cl.[CH3:2][C:3]1[CH:8]=[C:7]([CH3:9])[CH:6]=[C:5]([CH3:10])[C:4]=1[NH:11][NH2:12].[CH3:13][CH2:14][C:15](=O)[CH2:16][C:17](=O)[CH2:18][CH3:19].C(N(CC)CC)C>C(O)C>[CH2:14]([C:15]1[CH:16]=[C:17]([CH2:18][CH3:19])[N:11]([C:4]2[C:3]([CH3:2])=[CH:8][C:7]([CH3:9])=[CH:6][C:5]=2[CH3:10])[N:12]=1)[CH3:13]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 819233,5-HeptanedioneHCID 27748831-Mesitylhydrazine hydrochloride

생성물 1

HCID 218373383,5-Diethyl-1-(2,4,6-trimethylphenyl)-1H-pyrazole수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 7.46 g (0.04 mol) of 2,4,6-trimethylphenylhydrazine hydrochloride, 5.12 g (0.40 mol) of 3,5-heptanedione and 4.18 mL (0.60 mol) of triethylamine in 100 mL of absolute ethanol was refluxed overnight. The solvent was evaporated from the cooled reaction mixture and the residues were partitioned between water and ethyl acetate. The organic extracts were dried with brine and magnesium sulfate, and the solvent was evaporated to give the desired product in 95% yield. This compound was used in the subsequent reaction without further purification 1H-NMR (CDCl3): 0.11 (3H, t, J=7), 1.24 (3H, t, J=7), 1.90 (6H, s), 2.22 (2H, q, J-7), 2.28 (3H, s), 2.65 ) (2H, q, J=7), 5.96 (1H, s), 6.86 (2H, s).

후처리

  1. customThe solvent was evaporated from the cooled reaction mixture
  2. customthe residues were partitioned between water and ethyl acetate
  3. dry with materialThe organic extracts were dried with brine and magnesium sulfate
  4. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-2886b1c7caa94998bbaa10383f0b9411
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705646

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