Water → 1-Isopropylaminocarbonyl-4-chloro-3-(3,5-dichlorophenyl)pyrazole

HRID 1586366ノート

反応式

HRID 1586366 の反応式
[CH:1]([N:4]=[C:5]=[O:6])([CH3:3])[CH3:2].[Cl:7][C:8]1[C:9]([C:13]2[CH:18]=[C:17]([Cl:19])[CH:16]=[C:15]([Cl:20])[CH:14]=2)=[N:10][NH:11][CH:12]=1.C(N(CC)CC)C.O>CN(C=O)C>[CH:1]([NH:4][C:5]([N:11]1[CH:12]=[C:8]([Cl:7])[C:9]([C:13]2[CH:14]=[C:15]([Cl:20])[CH:16]=[C:17]([Cl:19])[CH:18]=2)=[N:10]1)=[O:6])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 61277Isopropyl isocyanateHCID 178478181HCID 178478181、化合物

生成物 1

HCID 218526341-Isopropylaminocarbonyl-4-chloro-3-(3,5-dichlorophenyl)pyrazole収率 63.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.95 g (0.011 mol) of isopropyl isocyanate are added, dropwise and at 0° C., to a solution of 2.55 g (0.01 mol) of 4-chloro-3-(3,5-dichlorophenyl)-1H-pyrazole and 1.55 ml (0.011 mol) of triethylamine in 20 ml of anhydrous DMF. Stirring is continued for 2 h at room temperature. The reaction mixture is poured into 100 ml of water and extracted with ethyl acetate. After drying the organic phase and concentration under vacuum, the residue is triturated with 50 ml of heptane, filtered and dried. We obtain 2.10 g of 1-isopropylaminocarbonyl-4-chloro-3-(3,5-dichlorophenyl)pyrazole, melting at 127° C.

後処理

  1. customat 0° C.
  2. extractionextracted with ethyl acetate
  3. customAfter drying
  4. concentrationthe organic phase and concentration under vacuum
  5. customthe residue is triturated with 50 ml of heptane
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-850f7cfbe8cf44ea8b8fe1a5760a2a29
出典データセット
uspto-grants-1999_08
特許番号
US05945382

反応ノート

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