Sodium Azide → HCID 86625618、化合物

HRID 14508ノート

反応式

HRID 14508 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 86625618HCID 86625618、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-227e4f63db1f4277a6ca3bc5b60605a5
出典データセット
uspto-grants-2010_06
特許番号
US07732435B2

反応ノート

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