Sodium Carbonate → HCID 13067124, 화합물

HRID 647633노트

반응식

HRID 647633 반응식
P(Cl)(Cl)(Cl)=O.[Cl:6][C:7]1[CH:28]=[CH:27][C:10]2[C:11]3[C:12](=[CH:23][NH:24][C:25]=3[CH3:26])[CH2:13][N:14]=[C:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[Cl:22])[C:9]=2[CH:8]=1.[C:29](=O)([O-])[O-:30].[Na+].[Na+]>CN(C)C=O>[Cl:6][C:7]1[CH:28]=[CH:27][C:10]2[C:11]3[C:12](=[C:23]([CH:29]=[O:30])[NH:24][C:25]=3[CH3:26])[CH2:13][N:14]=[C:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[Cl:22])[C:9]=2[CH:8]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 13067111HCID 13067111, 화합물

생성물 1

HCID 13067124HCID 13067124, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

By means of a syringe 0.6 ml (6.5 mmol) of phosphorous oxychloride was added to a solution of 0.7 g (2.0 mmol) of 8-chloro-6-(2-chlorophenyl)-1-methyl-2H,4H-pyrrolo[3,4-d][2]benzazepine in 8 ml of dimethylformamide which was cooled to 0°. The mixture was stirred at 0° for 1 hr, poured into 50 ml of saturated aqueous sodium carbonate and extracted with methylene chloride. The methylene chloride solution was washed with water, dried over anhydrous sodium sulfate and concentrated at reduced pressure to give a red amorphous solid. Purification by column chromatography (silica gel, 20 g; 4% ether in methylene chloride, eluent) gave an off-white solid. Recrystallization from a mixture of methylene chloride and ethyl acetate gave off-white crystals, mp 274°-276°.

후처리

  1. temperaturewas cooled to 0°
  2. extractionextracted with methylene chloride
  3. washThe methylene chloride solution was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated at reduced pressure
  6. customto give a red amorphous solid
  7. customPurification by column chromatography (silica gel, 20 g; 4% ether in methylene chloride, eluent)
  8. customgave an off-white solid
  9. customRecrystallization
  10. additionfrom a mixture of methylene chloride and ethyl acetate
  11. customgave off-white crystals, mp 274°-276°

출처 및 근거

ORD 기록
ord-c7e7163311df4aa4b7e6734a9d025890
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04409390

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