反応式
[N:1]([C:4](=[CH:10][C:11]1[CH:12]=[N:13][CH:14]=[CH:15][C:16]=1[O:17][CH3:18])[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[N+]=[N-]>CC1C=CC=CC=1C>[CH2:8]([O:7][C:5]([C:4]1[NH:1][C:12]2=[N:13][CH:14]=[CH:15][C:16]([O:17][CH3:18])=[C:11]2[CH:10]=1)=[O:6])[CH3:9]参加物
3
実験手順
A stirred solution of ethyl-α-azido-β-(4-methoxypyrid-3-yl)-acrylate 2 (3.7 g, 14.9 mmol) in dry o-xylene (35 mL) was heated in an oil bath at 170° C. for 25 min. During this time the contents of the flask gained brick red color. After cooling, the mixture was concentrated under high vacuum. The resultant brown residue was purified on silica gel column using 5% methanol in CH2Cl2 to give 3 as brick red solid. Mp 195-197° C.; Yield: 3.3 g, 82%; ESI MS: m/z 220.9 (M+1).
後処理
- temperatureAfter cooling
- concentrationthe mixture was concentrated under high vacuum
- customThe resultant brown residue was purified on silica gel column
- customto give 3 as brick red solid
出典と根拠
- ORDレコード
- ord-1feb00a08af34c57a4e5d752862b7d45
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07666898B2
関連ノート
読み込み中…