HCID 60046932, 화합물 → HCID 60046926, 화합물

HRID 1672310노트

반응식

HRID 1672310 반응식
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)=[C:7]([N+:12]([O-])=O)[CH:8]=[N:9]2)=[CH:4][CH:3]=1>C1COCC1.CO.[Ni]>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)=[C:7]([NH2:12])[CH:8]=[N:9]2)=[CH:4][CH:3]=1

참가 물질

4

반응물 1

HCID 60046932HCID 60046932, 화합물

생성물 1

HCID 60046926HCID 60046926, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

1.3 g (4.09 mmol) (7-chloro-3-nitro-quinolinyl)-(4-fluoro-phenyl)-amine (Example 15c) in 60 ml THF/MeOH 2:1 and 0.6 g Raney-Ni are hydrogenated at rt for 2 h. The reaction solution is filtered on Hyflo® Super Cel diatomaceous earth and is evaporated to dryness. The raw product is dissolved in 30 ml ethyl acetate, and ca. 400 ml hexane are added. The title compound precipitates and is collected by filtration. Drying follows at 65° C. over night. mp: 198-200° C.; MS: 288 (M++1); HPLC: tret=8.38 min (Grad 1).

후처리

  1. filtrationThe reaction solution is filtered on Hyflo® Super Cel diatomaceous earth
  2. customis evaporated to dryness
  3. dissolutionThe raw product is dissolved in 30 ml ethyl acetate
  4. additionca. 400 ml hexane are added
  5. customThe title compound precipitates
  6. filtrationis collected by filtration
  7. customDrying
  8. waitfollows at 65° C. over night
  9. customtret=8.38 min (Grad 1)

출처 및 근거

ORD 기록
ord-6f10e01e9c58416595f962f1bd2d17a4
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998972B2

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