4-Fluoroaniline → HCID 60046932, 화합물

HRID 1672309노트

반응식

HRID 1672309 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([Cl:12])=[CH:9][CH:10]=2)[N:5]=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].[F:16][C:17]1[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=1>O>[Cl:12][C:8]1[CH:7]=[C:6]2[C:11]([C:2]([NH:21][C:20]3[CH:22]=[CH:23][C:17]([F:16])=[CH:18][CH:19]=3)=[C:3]([N+:13]([O-:15])=[O:14])[CH:4]=[N:5]2)=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 97314-FluoroanilineHCID 534398754,7-Dichloro-3-nitroquinoline

생성물 1

HCID 60046932HCID 60046932, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.3 g (5.3 mmol) 4,7-dichloro-3-nitro-quinoline (Example 15b) and 0.525 g (5.3 mmol) 4-fluoroaniline are stirred at rt for 1 h. The reaction mixture is poured into 150 ml of water, and the resulting crystals are filtered off. After washing with water, the solid is dissolved in ca. 170 ml of ethanol and then concentrated to ca. 30 ml. The solution is cooled in ice-water. The crystals which precipitate are filtered off and dried overnight at 70° C. (high vacuum). mp: 198-200° C.; MS: 318 (M++1); HPLC: tret=10.92 min (Grad 1).

후처리

  1. filtrationthe resulting crystals are filtered off
  2. washAfter washing with water
  3. dissolutionthe solid is dissolved in ca. 170 ml of ethanol
  4. concentrationconcentrated to ca. 30 ml
  5. temperatureThe solution is cooled in ice-water
  6. filtrationThe crystals which precipitate are filtered off
  7. customdried overnight at 70° C. (high vacuum)
  8. customtret=10.92 min (Grad 1)

출처 및 근거

ORD 기록
ord-ace51838c99e490f8f2c6e54d9902c88
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998972B2

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