Carbon Tetrachloride → 3-bromo-1-methyl-5-phenyl-1H-1,5-benzodiazepine-2,4-(3H, 5H)-dione

HRID 704556ノート

反応式

HRID 704556 の反応式
[Br:1]Br.C(Cl)(Cl)(Cl)Cl.[CH3:8][N:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:12](=[O:26])[CH2:11][C:10]1=[O:27]>C(Cl)Cl>[Br:1][CH:11]1[C:10](=[O:27])[N:9]([CH3:8])[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:12]1=[O:26]

参加物

5

反応物 3

HCID 5943Carbon Tetrachloride2 回HCID 24408BromineHCID 146976571-Methyl-5-phenyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione

生成物 1

HCID 146976583-bromo-1-methyl-5-phenyl-1H-1,5-benzodiazepine-2,4-(3H, 5H)-dione

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

While irradiating with a 500 watt lamp at about 40° C., a solution of 5 ml of bromine and 30 ml of carbon tetrachloride was introduced dropwise into a solution of 25 g of the product of Step A and 750 ml of carbon tetrachloride. At the end of the introduction, the lamp was extinguished, the mixture was cooled and 500 ml of methylene chloride were added. The organic phase was washed with a saturated sodium carbonate solution, then with water and the product obtained was chromatographed on silica. Elution with an ethyl acetate-methylene chloride mixture 7-3-yielded 10.5 g of the sought product melting at 132° C.

後処理

  1. customWhile irradiating with a 500 watt lamp at about 40° C.
  2. temperaturethe mixture was cooled
  3. washThe organic phase was washed with a saturated sodium carbonate solution
  4. customwith water and the product obtained
  5. customwas chromatographed on silica
  6. washElution with an ethyl acetate-methylene chloride mixture 7-3-yielded 10.5 g of the sought product melting at 132° C.

出典と根拠

ORDレコード
ord-7b5917404f58451d91da8598e69df656
出典データセット
uspto-grants-1991_01
特許番号
US04988692

反応ノート

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