Dimethylamine → HCID 20379981、化合物

HRID 1658669ノート

反応式

HRID 1658669 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:32])[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18]([OH:31])([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.[CH3:33][NH:34][CH3:35]>CS(C)=O>[CH3:33][N:34]([CH3:35])[C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:32])[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18]([OH:31])([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:14][CH2:13]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 206183HCID 206183、化合物

生成物 1

HCID 20379981HCID 20379981、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

Through a solution of 18 g (0.041 mole) of 4'-fluoro-4-[4-(α-hydroxy-α-phenylbenzyl)piperidino]butyrophenone in 150 ml of dimethylsulfoxide (DMSO) was vigorously bubbled dimethylamine for 6 hours at 100°C. Most of the DMSO was removed at reduced pressure and a temperature of 120°C. The remaining mixture was poured into water and sodium carbonate to which was added a small amount of methanol. The resulting solid was filtered and dissolved in warm methanol and isopropyl alcohol, treated with charcoal filtered, and cooled. The solid which formed upon cooling was filtered off and recrystallized from acetone-heptane to give the desired product, M.P. 148°-150°C.

後処理

  1. customfor 6 hours
  2. customat 100°C
  3. customMost of the DMSO was removed at reduced pressure
  4. customa temperature of 120°C
  5. additionThe remaining mixture was poured into water and sodium carbonate to which
  6. additionwas added a small amount of methanol
  7. filtrationThe resulting solid was filtered
  8. dissolutiondissolved in warm methanol
  9. additionisopropyl alcohol, treated with charcoal
  10. filtrationfiltered
  11. temperaturecooled
  12. customThe solid which formed
  13. temperatureupon cooling
  14. filtrationwas filtered off
  15. customrecrystallized from acetone-heptane

出典と根拠

ORDレコード
ord-267a52e876d9415a907a57d373f19522
出典データセット
uspto-grants-1976_06
特許番号
US03965257

反応ノート

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