Hydrogen Peroxide → HCID 13280945、化合物

HRID 1903631ノート

反応式

HRID 1903631 の反応式
OO.S(=O)(=O)(O)O.[Cl:8][C:9]1[CH:31]=[CH:30][C:12]2[C:13]3[C:14](=[CH:25][N:26]([CH3:29])[C:27]=3[CH3:28])[CH2:15][N:16]=[C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:24])[C:11]=2[CH:10]=1.S(=O)(O)[O-:33].[Na+]>C(O)(=O)C>[Cl:8][C:9]1[CH:31]=[CH:30][C:12]2[C:13]3[CH:27]([CH3:28])[N:26]([CH3:29])[C:25](=[O:33])[C:14]=3[CH2:15][N:16]=[C:17]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[Cl:24])[C:11]=2[CH:10]=1

参加物

6

反応物 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 13280935HCID 13280935、化合物HCID 23665763Sodium Bisulfite

生成物 1

HCID 13280945HCID 13280945、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In one portion, 0.7 ml (5.9 mmol) of a 30% hydrogen peroxide solution was added to 33 ml of a 1% solution of concentrated sulfuric acid in acetic acid. After stirring for 1 hour, 1.8 g (5.0 mmol) of 8-chloro-6-(2-chlorophenyl)-1,2-dimethyl-2H,4H-pyrrolo[3,4-d][2]benzazepine were added, and the resulting solution was stirred for 20 minutes. The excess peracid was discharged by the addition of saturated aqueous sodium bisulfite solution, and the mixture was concentrated at reduced pressure. The residue was partitioned between methylene chloride and water and basififed with concentrated ammonium hydroxide solution. The methylene chloride solution was washed with brine, dried over anhydrous sodium sulfate and concentrated at reduced pressure to a yellow residue. Crystallization from ethyl aceatate gave 8-chloro-6-(2-chlorophenyl)-1,4-dihydro-1,2-dimethylpyrrolo[3,4-d][2]benzazepin-3(2H)-one as pale yellow prisms, mp 207°-208° C.

後処理

  1. stirringthe resulting solution was stirred for 20 minutes
  2. concentrationthe mixture was concentrated at reduced pressure
  3. customThe residue was partitioned between methylene chloride and water and basififed with concentrated ammonium hydroxide solution
  4. washThe methylene chloride solution was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated at reduced pressure to a yellow residue
  7. customCrystallization from ethyl aceatate

出典と根拠

ORDレコード
ord-c4460e0a50f84967862d9fd13aee9c2b
出典データセット
uspto-grants-1984_03
特許番号
US04436662

反応ノート

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