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HCID 13687205, 화합물 → HCID 13687203, 화합물

HRID 1731987
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HRID 1731987 반응식
[Cl:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([N:11]2[C:19]([CH3:20])=[C:18]3[C:13]([CH2:14][CH2:15][CH2:16][CH2:17]3)=[N:12]2)=[C:4]([F:21])[CH:3]=1>C(O)(=O)C.C(OCC)(=O)C.[Fe]>[Cl:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([N:11]2[C:19]([CH3:20])=[C:18]3[C:13]([CH2:14][CH2:15][CH2:16][CH2:17]3)=[N:12]2)=[C:4]([F:21])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 13687205HCID 13687205, 화합물

생성물 1

HCID 13687203HCID 13687203, 화합물수율 99.6%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 176Acetic Acid용매2회HCID 8857Ethyl Acetate용매

실험 절차

A mixture of iron powder (3 g) and a 5% aqueous acetic acid solution (10 ml) was heated at 90° to 100° C. while stirring for 10 minutes. To the resulting mixture, there was dropwise added 2-(4-chloro-2-fluoro-5-nitrophenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole (2 g) in acetic acid (10 ml) and ethyl acetate (10 ml), followed by stirring at the same temperature for 1 hour. After cooling, the iron powder was eliminated by filtration, and the filtrate was extracted with ethyl acetate. The organic layer was washed with a saturated sodium bicarbonate solution, dried and concentrated. The crystallized residue was collected by filtration and washed with ether to obtain 1.8 g of 2-(4-chloro-2-fluoro-5-aminophenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole, m.p., 107°-108° C.

후처리

  1. stirringby stirring at the same temperature for 1 hour
  2. temperatureAfter cooling
  3. filtrationthe iron powder was eliminated by filtration
  4. extractionthe filtrate was extracted with ethyl acetate
  5. washThe organic layer was washed with a saturated sodium bicarbonate solution
  6. customdried
  7. concentrationconcentrated
  8. filtrationThe crystallized residue was collected by filtration
  9. washwashed with ether

출처 및 근거

ORD 기록
ord-907f08d51e9a49718494acd2c8001f5f
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04624699

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