Triethylamine → N-(4-phenylthiobenzyl)-4-chloro-3-ethyl-1-methyl-5-pyrazole carboxamide

HRID 2248377

反応式

HRID 2248377 の反応式
C(OCC)(=O)C.[C:7]1([S:13][C:14]2[CH:21]=[CH:20][C:17]([CH2:18][NH2:19])=[CH:16][CH:15]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C(N(CC)CC)C.CC1C=CC(OC2C=CC(CN[C:41]([C:43]3[N:47]([CH3:48])[N:46]=[C:45]([CH2:49][CH3:50])[C:44]=3[Cl:51])=[O:42])=CC=2)=CC=1>O>[C:7]1([S:13][C:14]2[CH:21]=[CH:20][C:17]([CH2:18][NH:19][C:41]([C:43]3[N:47]([CH3:48])[N:46]=[C:45]([CH2:49][CH3:50])[C:44]=3[Cl:51])=[O:42])=[CH:16][CH:15]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 10110536TolfenpyradHCID 12842469[4-(Phenylsulfanyl)phenyl]methanamine

生成物 1

HCID 15008488N-(4-phenylthiobenzyl)-4-chloro-3-ethyl-1-methyl-5-pyrazole carboxamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into 50 ml solution of ethyl acetate containing 3.50 g of 4-phenylthiobenzylamine and 2.2 g of triethylamine, was dropped 3.60 g of 4-chloro-3-ethyl-1-methyl-5-pyrazolecarboxylic acid chloride synthesized in Example 2. After the completion of dropping, the mixture was stirred for 1.5 hours, poured into iced water and then extracted with ethyl acetate. The ethyl acetate layer was washed with an aqueous solution of sodium carbonate, water and a saturated aqueous solution of sodium chloride. After drying over anhydrous sodium sulfate, the solution was concentrated under a reduced pressure. The residue was purified on silica gel column chromatography to obtain 4.70 g of the titled compound (No. 76) shown in Table 1.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with an aqueous solution of sodium carbonate, water
  3. dry with materialAfter drying over anhydrous sodium sulfate
  4. concentrationthe solution was concentrated under a reduced pressure
  5. customThe residue was purified on silica gel column chromatography

出典と根拠

ORDレコード
ord-043a92cc036548b794a77392fa9feb9c
出典データセット
uspto-grants-1991_08
特許番号
US05039693

関連ノート

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