Trimethylsilyldiazomethane → HCID 86669289、化合物
反応式
[CH3:1][Si](C=[N+]=[N-])(C)C.[Cl:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[C:11]([O:18][CH2:19][CH:20]([F:22])[F:21])[N:10]=1>CO.C(Cl)Cl>[CH3:1][O:14][C:13](=[O:15])[C:12]1[CH:16]=[CH:17][C:9]([Cl:8])=[N:10][C:11]=1[O:18][CH2:19][CH:20]([F:21])[F:22]参加物
5
実験手順
Trimethylsilyl diazomethane (2 M in hexane; 15.0 mL, 30.0 mmol) is added to a mixture of 6-chloro-2-(2,2-difluoro-ethoxy)-nicotinic acid (6.0 g, 25.3 mmol) in MeOH (50 mL) and DCM (100 mL). The reaction mixture is stirred at rt for 10 min, quenched with AcOH and concentrated. The residue is diluted with water and filtered. The filtercake is washed with water and dried at 40° C.
後処理
- customquenched with AcOH
- concentrationconcentrated
- additionThe residue is diluted with water
- filtrationfiltered
- washThe filtercake is washed with water
- customdried at 40° C.
出典と根拠
- ORDレコード
- ord-dd8e0126a1ee4d858b9efa63586726e5
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08586604B2
反応ノート
読み込み中…