Propane sultone → Agn-PC-004N6H

HRID 2219723ノート

反応式

HRID 2219723 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH:13]=2)=[CH:4][CH:3]=1.[CH2:14]1[CH2:20][S:17](=[O:19])(=[O:18])[O:16][CH2:15]1>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH2:13][CH2:12][N:11]([CH2:15][CH2:14][CH2:20][S:17]([OH:19])(=[O:18])=[O:16])[CH2:10][CH:9]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 14264Propane sultoneHCID 1977484-(4-Fluorophenyl)-1,2,3,6-tetrahydropyridine

生成物 1

HCID 11220282Agn-PC-004N6H

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 4-(4-fluorophenyl)-1,2,3,6-tetrahydropyridine (1.96 g, 13.7 mmol) in acetone (30 mL) was added 1,3-propane sultone (1.74 g, 14.5 mmol). The mixture was stirred at reflux overnight. Only a small amount of compound precipitated. The resulting suspension was cooled to room temperature with stirring and a larger amount of solid precipitated. The suspension was heated with the addition of a small amount of MeOH until complete dissolution of the solid. The resulting solution was stirred at reflux for a few minutes and was cooled to room temperature with stirring. The solid was collected by filtration, washed with MeOH and dried in vacuo. This allowed the isolation of compound F, 1.33 g (32%).

後処理

  1. temperatureat reflux overnight
  2. customOnly a small amount of compound precipitated
  3. stirringwith stirring
  4. customa larger amount of solid precipitated
  5. temperatureThe suspension was heated with the addition of a small amount of MeOH until complete dissolution of the solid
  6. stirringThe resulting solution was stirred
  7. temperatureat reflux for a few minutes
  8. temperaturewas cooled to room temperature
  9. stirringwith stirring
  10. filtrationThe solid was collected by filtration
  11. washwashed with MeOH
  12. customdried in vacuo

出典と根拠

ORDレコード
ord-c779a11bc7774e4cbe2b54faea188b3f
出典データセット
uspto-grants-2008_08
特許番号
US07414076B2

反応ノート

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