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Hydrochloric Acid → HCID 10061987, 화합물

HRID 1087182
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HRID 1087182 반응식
[CH3:1][N:2]([C:11]1[CH:12]=[C:13]([C:20]2([CH3:25])OCC[O:21]2)[CH:14]=[CH:15][C:16]=1[N+:17]([O-])=O)[C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:4]=1[F:10].Cl>CC(C)=O>[NH2:17][C:16]1[CH:15]=[CH:14][C:13]([C:20](=[O:21])[CH3:25])=[CH:12][C:11]=1[N:2]([CH3:1])[C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][C:4]=1[F:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 19817746HCID 19817746, 화합물

생성물 1

HCID 10061987HCID 10061987, 화합물수율 21.1%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 2-{3-[N-methyl-N-(2,4-difluorophenyl)amino]-4-nitrophenyl}-2-methyl-1,3-dioxolane (6.6 g) and 3N-hydrochloric acid (60 ml) in acetone (120 ml) was stirred at room temperature overnight and evaporated. The residue was dissolved in ethyl acetate, washed with water and an aqueous solution of sodium bicarbonate, and concentrated to dryness. A mixture of the residual oil (5.3 g), iron powder (5 g) and ammonium chloride (0.5 g) in ethanol (120 ml) and water (60 ml) was stirred and refluxed for 1 hour. The mixture was filtered and the filtrate was evaporated. The residue was purified by column chromatography on silica gel eluting with a mixture of toluene and ethyl acetate (20:1) to give crystals of 4'-amino-3'-[N-methyl-N-(2,4-difluorophenyl)amino]acetophenone (1.1 g).

후처리

  1. customevaporated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. concentrationan aqueous solution of sodium bicarbonate, and concentrated to dryness
  5. additionA mixture of the residual oil (5.3 g), iron powder (5 g) and ammonium chloride (0.5 g) in ethanol (120 ml) and water (60 ml)
  6. temperaturerefluxed for 1 hour
  7. filtrationThe mixture was filtered
  8. customthe filtrate was evaporated
  9. customThe residue was purified by column chromatography on silica gel eluting with a mixture of toluene and ethyl acetate (20:1)

출처 및 근거

ORD 기록
ord-76aae9ef7d8949d18f22b77eccbfaffa
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05034417

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