Acetonitrile → HCID 117902772、化合物

HRID 1772171ノート

反応式

HRID 1772171 の反応式
[CH3:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[N:5]2[CH:11]=1.[I:12]N1C(=O)CCC1=O.C(#N)C>C(Cl)Cl>[I:12][C:11]1[N:5]2[C:6]([CH3:10])=[CH:7][CH:8]=[CH:9][C:4]2=[N:3][C:2]=1[CH3:1]

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 120273N-IodosuccinimideHCID 1386822,5-Dimethylimidazo(1,2-a)pyridine

生成物 1

HCID 117902772HCID 117902772、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2,5-dimethylimidazo[1,2-a]pyridine (0.5 g, 3.4 mmol), N-iodosuccinimide (770 mg, 3.4 mmol) and ACN (5 ml) is stirred at RT for 45 minutes. The mixture is diluted with DCM and extracted with an aqueous solution sodium thiosulfate. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by RP HPLC. Yield: 775 mg (83%). HPLC-MS: M+H=273; tR=1.02 min (METHOD—1).

後処理

  1. extractionextracted with an aqueous solution sodium thiosulfate
  2. dry with materialThe combined organic layers are dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe product is purified by RP HPLC

出典と根拠

ORDレコード
ord-039d71eed34f48048ad1f5b66bb0b01a
出典データセット
uspto-grants-2016_02
特許番号
US09249151B2

反応ノート

読み込み中…