Sodium Azide → HCID 86625618, 화합물

HRID 14508노트

반응식

HRID 14508 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17](=[O:18])[C:16]3[C:11](=[CH:12][C:13](F)=[CH:14][CH:15]=3)[O:10][C:9]=2[CH:20]([CH3:22])[CH3:21])=[CH:4][CH:3]=1.[N-:23]=[N+:24]=[N-:25].[Na+]>CN(C)C=O>[N:23]([C:13]1[CH:12]=[C:11]2[C:16]([C:17](=[O:18])[C:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)=[C:9]([CH:20]([CH3:22])[CH3:21])[O:10]2)=[CH:15][CH:14]=1)=[N+:24]=[N-:25]

참가 물질

4

반응물 2

HCID 33557Sodium AzideHCID 686998323-(4-Chlorophenyl)-7-fluoro-2-isopropyl-chromen-4-one

생성물 1

HCID 86625618HCID 86625618, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

To a solution of 3-(4-chlorophenyl)-7-fluoro-2-isopropyl-chromen-4-one (4.0 g, 12.7 mmol) in dry dimethylformamide (120 ml) is added sodium azide at room temperature. The reaction mixture is heated at 90° C. for 16 h, cooled to room temperature and partitioned between ethyl acetate and water. The organic phase is washed with water and brine, dried (MgSO4) and concentrated in vacuo. Purification by flash chromatography on silica gel using iso-hexane:ethyl acetate (10:1) as the eluent, followed by recrystallisation from iso-hexane, gives the title compound.

후처리

  1. temperaturecooled to room temperature
  2. custompartitioned between ethyl acetate and water
  3. washThe organic phase is washed with water and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customPurification by flash chromatography on silica gel
  7. customfollowed by recrystallisation from iso-hexane

출처 및 근거

ORD 기록
ord-227e4f63db1f4277a6ca3bc5b60605a5
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732435B2

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