N-bromobutanimide → HCID 118021566、化合物
反応式
[CH3:1][N:2]1[CH:7]=[CH:6][C:5]2[CH2:8][CH2:9][CH2:10][C:4]=2[C:3]1=[O:11].C1C(=O)N([Br:19])C(=O)C1>C(#N)C>[Br:19][C:6]1[C:5]2[CH2:8][CH2:9][CH2:10][C:4]=2[C:3](=[O:11])[N:2]([CH3:1])[CH:7]=1参加物
4
実験手順
The title compound of step 6 (140 mg, 1.04 mmol) was dissolved in ACN (5 mL) and NBS (188 mg, 1.06 mmol) was added. After stirring at rt for 1.5 h, purification by silica gel chromatography (PE/EtOAc=1:1) gave the title compound (196 mg, 89.5%) as a white solid. 1H NMR (CD3Cl, 300 MHz): δ 7.33 (s, 1H), 3.53 (s, 3H), 2.85-2.97 (m, 4H), 2.05-2.13 (m, 2H). LCMS: 228, 230 (M+1)+
後処理
- custompurification by silica gel chromatography (PE/EtOAc=1:1)
出典と根拠
- ORDレコード
- ord-1fd592006b5e4cdbb50c72b6aae32214
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09034900B2
反応ノート
読み込み中…