Sodium Carbonate → HCID 13067124、化合物

HRID 2296289ノート

反応式

HRID 2296289 の反応式
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

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 13067111HCID 13067111、化合物

生成物 1

HCID 13067124HCID 13067124、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-b79679c127f546d2955431e397bb18d2
出典データセット
uspto-grants-1984_01
特許番号
US04428878

反応ノート

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