Dichloromethane → HCID 82004536、化合物
反応式
[H-].[Na+].[F:3][CH:4]([F:7])[CH2:5][OH:6].C(Cl)Cl.Cl[C:12]1[N:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=[O:15]>O.C1COCC1>[Cl:21][C:19]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[C:12]([O:6][CH2:5][CH:4]([F:7])[F:3])[N:20]=1参加物
7
実験手順
NaH (55% dispersion in oil; 5.0 g, 114.6 mmol) is added portionwise at 10° C. to 2,2-difluoroethanol (6.25 mL, 99.0 mmol), DCM (200 mL) and THF (75 mL). After 10 min 2,6-dichloro-nicotinic acid (5.0 g, 24.7 mmol) is added to the reaction mixture and it is stirred at rt overnight. Then water is added and it is concentrated. The residue is diluted with water and extracted with Et2O. Formic acid is added to the aqueous layers the precipitate is filtered off, washed with water and dried to give the sub-title compound.
後処理
- concentrationit is concentrated
- additionThe residue is diluted with water
- extractionextracted with Et2O
- additionFormic acid is added to the aqueous layers the precipitate
- filtrationis filtered off
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-3f92e20ce98a4fbfa134fc2bc4e3256f
- 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…