HCID 60046932、化合物 → HCID 60046926、化合物

HRID 1672310ノート

反応式

HRID 1672310 の反応式
[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

参加物

4

反応物 1

HCID 60046932HCID 60046932、化合物

生成物 1

HCID 60046926HCID 60046926、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6f10e01e9c58416595f962f1bd2d17a4
出典データセット
uspto-grants-2011_08
特許番号
US07998972B2

反応ノート

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