N-Iodosuccinimide → HCID 178447244、化合物
反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[NH:5][C:4]2=[N:15][CH:16]=[CH:17][C:3]=12.[I:18]N1C(=O)CCC1=O>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:11])[CH3:12])[NH:5][C:4]2=[N:15][CH:16]=[C:17]([I:18])[C:3]=12参加物
4
実験手順
4-Chloro-2-trimethylacetamido-pyrrolo[2,3-d]pyrimidine (9a, 10.9 g, 43.24 mmol) was dissolved in anhydrous THF (120 mL) under nitrogen. After the addition of N-iodosuccinimide (10.7 g, 47.56 mmol), the mixture was stirred at RT for 1 h. The solvent was then removed in vacuo. The residue dissolved in EtOAc (100 mL) and washed with 1 M sodium thiosulfate (3×100 mL). Column chromatography purification (2% MeOH in DCM, isocratic) yielded 9b (12.9 g).
後処理
- customThe solvent was then removed in vacuo
- dissolutionThe residue dissolved in EtOAc (100 mL)
- washwashed with 1 M sodium thiosulfate (3×100 mL)
- customColumn chromatography purification (2% MeOH in DCM, isocratic)
出典と根拠
- ORDレコード
- ord-163d365933ab4db29d548a7573a926bc
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08212020B2
反応ノート
読み込み中…