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

HRID 1586366노트

반응식

HRID 1586366 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 61277Isopropyl isocyanateHCID 178478181HCID 178478181, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-850f7cfbe8cf44ea8b8fe1a5760a2a29
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05945382

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