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

HRID 2248377

반응식

HRID 2248377 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-043a92cc036548b794a77392fa9feb9c
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05039693

연결된 노트

불러오는 중…