Bromine → HCID 20449986、化合物

HRID 358058ノート

反応式

HRID 358058 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH:12]=[N:13][N:14]=[C:10]3[CH2:9][CH:8]=[C:7]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[F:21])[C:6]=2[CH:22]=1.[Br:23]Br>C(Cl)(Cl)Cl.N1C=CC=CC=1>[Br:23][C:12]1[N:11]2[C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:22][C:6]=3[C:7]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[F:21])=[CH:8][CH2:9][C:10]2=[N:14][N:13]=1

参加物

5

反応物 2

HCID 24408BromineHCID 20449965HCID 20449965、化合物

生成物 1

HCID 20449986HCID 20449986、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒

実験手順

8.5 g of 8-chloro-6-(2-fluorophenyl)-4H-s-triazolo[4,3-a][1]benzazepine are dissolved in 135 ml of chloroform and 3.3 ml of pyridine. 2.0 ml of bromine are added dropwise at room temperature while stirring. The mixture is then heated to 55°-60° for 50 minutes and evaporated in vacuo. The residue is chromatographed on 550 g of silica gel. By elution with chloroform which contains 0.3% or 0.4% methanol and crystallization of the obtained material from benzene there is obtained 1-bromo-8-chloro-6-(2-fluorophenyl)-4H-s-triazolo[4,3-a][1]benzazepine of melting point 222°.

後処理

  1. temperatureThe mixture is then heated to 55°-60° for 50 minutes
  2. customevaporated in vacuo
  3. customThe residue is chromatographed on 550 g of silica gel
  4. washBy elution with chloroform which
  5. custom0.3% or 0.4% methanol and crystallization of the obtained material from benzene

出典と根拠

ORDレコード
ord-f17304d2dec14fe1b88b63b717520cc4
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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