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Aniline → N-[[[4-(6-bromo-1,3-benzodioxan-2-yl)phenyl]amino]carbonyl]-2,6,-difluorobenzamide

HRID 1708176
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HRID 1708176 반응식
[Br:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][CH:7]([C:10]3[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][CH:11]=3)[O:8][CH2:9][C:4]=2[CH:3]=1.[H][H].C(=O)([O-])[O-].[K+].[K+].NC1C=CC=CC=1.[F:36][C:37]1[CH:47]=[CH:46][CH:45]=[C:44]([F:48])[C:38]=1[C:39]([N:41]=[C:42]=[O:43])=[O:40]>C1(C)C=CC=CC=1.[Pt]>[Br:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][CH:7]([C:10]3[CH:15]=[CH:14][C:13]([NH:16][C:42]([NH:41][C:39](=[O:40])[C:38]4[C:44]([F:48])=[CH:45][CH:46]=[CH:47][C:37]=4[F:36])=[O:43])=[CH:12][CH:11]=3)[O:8][CH2:9][C:4]=2[CH:3]=1
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참가 물질

8

반응물 5

HCID 6115AnilineHCID 11430Potassium CarbonateHCID 27333692,6-Difluorobenzoyl isocyanateHCID 189611956-Bromo-2-(4-nitrophenyl)-1,3-benzodioxanHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 18961193N-[[[4-(6-bromo-1,3-benzodioxan-2-yl)phenyl]amino]carbonyl]-2,6,-difluorobenzamide

시약·촉매·용매 2

HCID 23939Platinum촉매HCID 1140Toluene용매2회

반응 조건

온도
60 °C

실험 절차

A suspension of 6-bromo-2-(4-nitrophenyl)-1,3-benzodioxan (2.05 g) in toluene (150 ml) was hydrogenated at ≤60 psi hydrogen pressure in the presence of 5% platinum/charcoal (0.5 g) and anhydrous potassium carbonate (0.5 g) at ambient temperature. The reaction mixture was filtered and evaporated under reduced pressure, azeotropically removing the water formed in the reaction. The resulting crude aniline derivative was redissolved in dry toluene (25 ml) and treated with 2,6-difluorobenzoyl isocyanate (1.2 g), warming briefly to approx. 60° C. then allowing the stirred reaction mixture to cool overnight. Cooling to 0°-5° C. afforded a precipitate of impure product which was purified by crystallisation from ethanol (0.52 g, 17%), mp 194°-195° C.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customevaporated under reduced pressure
  3. customazeotropically removing the water
  4. customformed in the reaction
  5. customthe stirred reaction mixture
  6. temperatureto cool overnight
  7. temperatureCooling to 0°-5° C.
  8. customafforded a precipitate of impure product which
  9. customwas purified by crystallisation from ethanol (0.52 g, 17%), mp 194°-195° C.

출처 및 근거

ORD 기록
ord-c76d30b020a842a4b830bb5e106f322f
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05356924

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