Bromine → HCID 20450024、化合物

HRID 358071ノート

反応式

HRID 358071 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:12](=[O:15])[NH:13][N:14]=[C:10]3[CH2:9][CH2:8][CH:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1.BrBr>C(Cl)(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:12](=[O:15])[NH:13][N:14]=[C:10]3[CH2:9][CH:8]=[C:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1

参加物

4

反応物 2

HCID 24408BromineHCID 20449987HCID 20449987、化合物

生成物 1

HCID 20450024HCID 20450024、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A suspension of 660 mg of 8-chloro-6-(2-fluorophenyl)-2,4,5,6-tetrahydro-1H-s-triazolo[4,3-a][1]benzazepin-1-one in 150 ml of carbon tetrachloride is treated with 0.11 ml of bromine and heated to boiling while stirring for 2 hours while irradiating with a 500 W incandescent lamp. The solution is evaporated in vacuo. The residue is dissolved in chloroform and the solution is washed twice with saturated sodium hydrogen carbonate solution, dried and evaporated in vacuo. The residue is chromatographed on 35 g of silica gel. By elution with toluene/ethyl acetate (4:1) and crystallization from ethyl acetate/ether there is obtained 8-chloro-6-(2-fluorophenyl)-2,4-dihydro-1H-s-triazolo[4,3-a][1]benzazepin-1-one of melting point 221°-224°.

後処理

  1. temperatureheated
  2. customwhile irradiating with a 500 W incandescent lamp
  3. customThe solution is evaporated in vacuo
  4. dissolutionThe residue is dissolved in chloroform
  5. washthe solution is washed twice with saturated sodium hydrogen carbonate solution
  6. customdried
  7. customevaporated in vacuo
  8. customThe residue is chromatographed on 35 g of silica gel
  9. washBy elution
  10. customwith toluene/ethyl acetate (4:1) and crystallization from ethyl acetate/ether there

出典と根拠

ORDレコード
ord-5737726de2d348dc8825c65b16dd33cf
出典データセット
uspto-grants-1984_08
特許番号
US04464300

反応ノート

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