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Tetrahydrofuran → 3-(3-Fluoro-5-chloro-2-pyridyl)-4-amino-5difluoromethoxy-1-methyl-[1H]-pyrazole

HRID 1532581
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HRID 1532581 반응식
[F:1][C:2]1[C:3]([C:9]2[C:13]([N+:14]([O-])=O)=[C:12]([O:17][CH:18]([F:20])[F:19])[N:11]([CH3:21])[N:10]=2)=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.O1CCCC1.[H][H]>[Ni].C(O)C>[F:1][C:2]1[C:3]([C:9]2[C:13]([NH2:14])=[C:12]([O:17][CH:18]([F:19])[F:20])[N:11]([CH3:21])[N:10]=2)=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8028TetrahydrofuranHCID 220135653-(3-Fluoro-5-chloro-2-pyridyl)-4-nitro-5-difluoromethoxy-1-methyl-[1H]-pyrazoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 220135593-(3-Fluoro-5-chloro-2-pyridyl)-4-amino-5difluoromethoxy-1-methyl-[1H]-pyrazole

시약·촉매·용매 2

HCID 935Nickel촉매
HCID 702
Ethanol
용매

실험 절차

4.2 g of 3-(3-fluoro-5-chloro-2-pyridyl)-4-nitro-5-difluoromethoxy-1-methyl-[1H]-pyrazole (Example H47) are initially introduced into the reaction vessel together with 40 ml of tetrahydrofuran, and 5.8 g of Raney nickel in ethanol are added. Hydrogenation is carried out under normal pressure and at a temperature of 30-35° C. After uptake of 728 ml of hydrogen, the hydrogenation is interrupted and the reaction mixture is filtered over Hyflo. After removal of the solvent in vacuo, 3.15 g of the desired title compound are obtained as a brown solid of melting point 92-94° C.

후처리

  1. additionare added
  2. customis carried out under normal pressure and at a temperature of 30-35° C
  3. filtrationthe reaction mixture is filtered over Hyflo
  4. customAfter removal of the solvent in vacuo, 3.15 g of the desired title compound
  5. customare obtained as a brown solid of melting point 92-94° C.

출처 및 근거

ORD 기록
ord-5e58418e08774547a7d15f032556f7af
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06204221B1

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