Triethylamine → HCID 89996006、化合物

HRID 1480835ノート

反応式

HRID 1480835 の反応式
[CH3:1][N:2]1[CH:6]=[C:5]([C:7]2[N:16]=[CH:15][CH:14]=[C:13]3[C:8]=2[CH:9]=[C:10]([OH:17])[N:11]=[CH:12]3)[CH:4]=[N:3]1.[O:18](S(C(F)(F)F)(=O)=O)[S:19]([C:22]([F:25])([F:24])[F:23])(=O)=[O:20].C(N(CC)CC)C>C(Cl)Cl>[F:23][C:22]([F:25])([F:24])[S:19]([O:17][C:10]1[N:11]=[CH:12][C:13]2[C:8]([CH:9]=1)=[C:7]([C:5]1[CH:4]=[N:3][N:2]([CH3:1])[CH:6]=1)[N:16]=[CH:15][CH:14]=2)(=[O:20])=[O:18]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 67749Trifluoromethanesulfonic anhydrideHCID 178480127HCID 178480127、化合物

生成物 1

HCID 89996006HCID 89996006、化合物収率 59.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-(1-methyl-1H-pyrazol-4-yl)-2,6-naphthyridin-3-ol (Preparation 89, 15 mg, 0.066 mmol) in DCM (0.5 mL) was added Tf2O (0.013 mL, 0.080 mmol) and triethylamine (9.3 uL, 0.066 mmol). The reaction mixture was stirred at room temperature under 1 hour. The reaction mixture was concentrated in vacuo. The residue was passed through a SCX-2 cartridge eluting with 100% MeOH—1M NH3 in MeOH to give the title compound (14 mg, 59%).

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. washeluting with 100% MeOH—1M NH3 in MeOH

出典と根拠

ORDレコード
ord-1f2812c9063c446cb3e92e33b2ad03f1
出典データセット
uspto-grants-2016_08
特許番号
US09409907B2

反応ノート

読み込み中…