Phosgene → HCID 20450024、化合物

HRID 358061ノート

反応式

HRID 358061 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:12][NH2:13])[CH2:9][CH:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])[C:6]=2[CH:21]=1.[C:22](Cl)(Cl)=[O:23]>N1C=CC=CC=1.C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:22](=[O:23])[NH:13][N:12]=[C:10]3[CH2:9][CH:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[F:20])[C:6]=2[CH:21]=1

参加物

5

反応物 2

HCID 6371PhosgeneHCID 20449973HCID 20449973、化合物

生成物 1

HCID 20450024HCID 20450024、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 1140Toluene溶媒

実験手順

0.15 g of 7-chloro-5-(2-fluorophenyl)-2-hydrazino-3H-1-benzazepine is dissolved in 10 ml of pyridine and treated with 1.44 ml of a 14.3% solution of phosgene in toluene. The mixture is heated to 60° for 5 minutes and then evaporated in vacuo. The residue is partitioned between benzene and water. The benzene phase is washed successively with water, with sodium hydrogen carbonate solution and with water. The solvent is evaporated in vacuo. The residue is chromatographed on 15 g of silica gel while eluting with benzene/ethyl acetate (19:1 and 9:1). After recrystallization from ether/hexane, there is obtained pure 8-chloro-6-(2-fluorophenyl)-2,4-dihydro-1H-s-triazolo[4,3-a][1]benzazepin-1-one of melting point 223°-225°.

後処理

  1. temperatureThe mixture is heated to 60° for 5 minutes
  2. customevaporated in vacuo
  3. customThe residue is partitioned between benzene and water
  4. washThe benzene phase is washed successively with water, with sodium hydrogen carbonate solution and with water
  5. customThe solvent is evaporated in vacuo
  6. customThe residue is chromatographed on 15 g of silica gel
  7. washwhile eluting with benzene/ethyl acetate (19:1 and 9:1)
  8. customAfter recrystallization from ether/hexane

出典と根拠

ORDレコード
ord-6b4689f3149c44fa96782260fb471bcb
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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