Bromine → HCID 20449986, 화합물

HRID 358058노트

반응식

HRID 358058 반응식
[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

참가 물질

5

반응물 2

HCID 24408BromineHCID 20449965HCID 20449965, 화합물

생성물 1

HCID 20449986HCID 20449986, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6212Chloroform용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-f17304d2dec14fe1b88b63b717520cc4
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04464300

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