Dimethylformamide → HCID 57551827、化合物

HRID 907333ノート

反応式

HRID 907333 の反応式
P(Cl)(Cl)(Cl)=O.[Br:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[N:12]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([CH3:28])(=[O:27])=[O:26])=[CH:21][CH:20]=1)[CH:11]=[CH:10]2.CN([CH:32]=[O:33])C>>[Br:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[N:12]([CH2:18][C:19]1[CH:24]=[CH:23][C:22]([S:25]([CH3:28])(=[O:26])=[O:27])=[CH:21][CH:20]=1)[CH:11]=[C:10]2[CH:32]=[O:33]

参加物

4

反応物 3

HCID 6228Dimethylformamide2 回HCID 24813Phosphorus oxychlorideHCID 575517876-Bromo-2-(4-methanesulfonyl-benzyl)-2H-isoquinolin-1-one

生成物 1

HCID 57551827HCID 57551827、化合物

実験手順

DMF (10 mL) was cooled in an ice bath and phosphorus oxychloride (1.4 mL) added over 20 seconds. The solution was stirred for 10 minutes at room temperature then a solution of the product of step i) (2.0 g) in DMF (4 mL) was added over 5 minutes. The mixture was heated at 95° C. for 16 hours then allowed to cool and poured onto ice/water. The mixture was then extracted into ethyl acetate (100 mL) the organics combined and evaporated under reduced pressure. The residue was purified (SiO2 chromatography, eluting with 1:1 ethyl acetate:isohexane) to give the sub-titled compound (1.5 g).

後処理

  1. temperatureThe mixture was heated at 95° C. for 16 hours
  2. temperatureto cool
  3. additionpoured onto ice/water
  4. extractionThe mixture was then extracted into ethyl acetate (100 mL) the
  5. customevaporated under reduced pressure
  6. customThe residue was purified
  7. wash(SiO2 chromatography, eluting with 1:1 ethyl acetate:isohexane)

出典と根拠

ORDレコード
ord-481810dd02aa4214b9f2b4c564e2f059
出典データセット
uspto-grants-2011_09
特許番号
US08012979B2

反応ノート

読み込み中…