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

HRID 725276ノート

反応式

HRID 725276 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2886b1c7caa94998bbaa10383f0b9411
出典データセット
uspto-grants-1998_01
特許番号
US05705646

反応ノート

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