Pyrazole → 1-(N-(2-isopropylvinyl)-N-tert.-butylcarbamyl)-pyrazole

HRID 1762857노트

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HRID 1762857 반응식
[NH:1]1[CH:5]=[CH:4][CH:3]=[N:2]1.[CH:6]([CH:9]=[CH:10][N:11]([C:15]([CH3:18])([CH3:17])[CH3:16])[C:12](Cl)=[O:13])([CH3:8])[CH3:7].C(=O)([O-])[O-].[K+].[K+]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH:6]([CH:9]=[CH:10][N:11]([C:15]([CH3:17])([CH3:16])[CH3:18])[C:12]([N:1]1[CH:5]=[CH:4][CH:3]=[N:2]1)=[O:13])([CH3:8])[CH3:7]

참가 물질

6

반응물 3

HCID 1048PyrazoleHCID 11430Potassium CarbonateHCID 56617464N-(2-isopropylvinyl)-N-tert.-butylcarbamyl chloride

생성물 1

HCID 566205451-(N-(2-isopropylvinyl)-N-tert.-butylcarbamyl)-pyrazole수율 64.4%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

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온도
40 °C

실험 절차

27.2 g (0.2 mole) of pyrazole, 1 g of 4-dimethylaminopyridine and 40.6 g (0.2 mole) of N-(2-isopropylvinyl)-N-tert.-butylcarbamyl chloride are added in succession to a suspension of 42 g of potassium carbonate in 150 ml of dry methylene chloride at 20° C. The mixture is stirred for 10 hours at 40° C., after which the resulting precipitate is filtered off under suction and washed with 200 ml of methylene chloride. The filtrate is washed with three times 80 ml of water, dried over Na2SO4 and evaporated down under reduced pressure, and the oil which remains is evaporated down under reduced pressure. 30.3 g of 1-(N-(2-isopropylvinyl)-N-tert.-butylcarbamyl)-pyrazole are obtained as a colorless liquid of boiling point 104°-105° C./0.3 mbar and nD 1.4828 (Compound No. 3).

후처리

  1. filtrationafter which the resulting precipitate is filtered off under suction
  2. washwashed with 200 ml of methylene chloride
  3. washThe filtrate is washed with three times 80 ml of water
  4. dry with materialdried over Na2SO4
  5. customevaporated down under reduced pressure
  6. customthe oil which remains is evaporated down under reduced pressure

출처 및 근거

ORD 기록
ord-bf9343b70db94b05abd91e64c1dd9577
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04835171

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