Hydrogen Peroxide → HCID 13280945, 화합물

HRID 1903631노트

반응식

HRID 1903631 반응식
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

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 13280935HCID 13280935, 화합물HCID 23665763Sodium Bisulfite

생성물 1

HCID 13280945HCID 13280945, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c4460e0a50f84967862d9fd13aee9c2b
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04436662

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