Bromine → HCID 20450024, 화합물

HRID 358071노트

반응식

HRID 358071 반응식
[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

참가 물질

4

반응물 2

HCID 24408BromineHCID 20449987HCID 20449987, 화합물

생성물 1

HCID 20450024HCID 20450024, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-5737726de2d348dc8825c65b16dd33cf
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04464300

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