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

HRID 1762857ノート

反応式

HRID 1762857 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

反応条件

温度
40 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-bf9343b70db94b05abd91e64c1dd9577
出典データセット
uspto-grants-1989_05
特許番号
US04835171

反応ノート

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