Trimethylsilyldiazomethane → HCID 68862597、化合物
反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]=1[C:12]([OH:14])=[O:13].[CH3:15][Si](C=[N+]=[N-])(C)C>C1C=CC=CC=1.CO>[CH3:15][C:11]1[C:2]([NH2:1])=[C:3]([C:12]([OH:14])=[O:13])[C:4]2[C:9]([CH:10]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2参加物
4
実験手順
2-Amino-1-naphthoic acid (3.21 g, 17.2 mmol) in 4:1 benzene/CH3OH (125 mL) was treated with trimethylsilyldiazomethane (9.0 mL, 18.0 mmol, 2.0M solution in hexanes), stirred for 2.5 hours, quenched with acetic acid (0.5 mL), and concentrated. The concentrate was purified by flash column chromatography (4:1 hexanes/ethyl acetate) to provide the desired compound (3.25 g). MS (ESI(+)) m/e 202 (M+H)+; (ESI(−)) m/e 200 (M−H)−.
後処理
- customquenched with acetic acid (0.5 mL)
- concentrationconcentrated
- customThe concentrate was purified by flash column chromatography (4:1 hexanes/ethyl acetate)
出典と根拠
- ORDレコード
- ord-7dc871bed0e2437c8bf18ae7a00d2045
- 出典データセット
- uspto-grants-2009_02
- 特許番号
- US07491718B2
反応ノート
読み込み中…