N-Iodosuccinimide → HCID 90104751、化合物

HRID 1049881ノート

反応式

HRID 1049881 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[N:8]=[C:9]3[CH:15]=[CH:14][NH:13][C:10]3=[N:11][CH:12]=2)=[CH:3][CH:2]=1.[I:16]N1C(=O)CCC1=O>CC(C)=O>[I:16][C:15]1[C:9]2[C:10](=[N:11][CH:12]=[C:7]([C:4]3[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=3)[N:8]=2)[NH:13][CH:14]=1

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 90105361HCID 90105361、化合物

生成物 1

HCID 90104751HCID 90104751、化合物収率 62.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

To a solution of 22 (0.35 g) and acetone (20 mL) of acetone was added in one portion N-iodosuccinimide (0.44 g). The mixture was stirred at RT for 30 min and then concentrated to afford 0.8 g of crude material. The crude product was purified by SiO2 chromatography eluting with and EtOH/EtOAc gradient (1 to 15% over 15 minutes) to afford 0.36 g of pure 7-iodo-2-(pyridin-4-yl)-5H-pyrrolo[2,3-b]pyrazine (24).

後処理

  1. concentrationconcentrated
  2. customto afford 0.8 g of crude material
  3. customThe crude product was purified by SiO2 chromatography
  4. washeluting with and EtOH/EtOAc gradient (1 to 15% over 15 minutes)

出典と根拠

ORDレコード
ord-58b569c93b6b4d5292b215fcec354392
出典データセット
uspto-grants-2016_07
特許番号
US09382257B2

反応ノート

読み込み中…