Potassium Phosphate, Tribasic → HCID 53373964、化合物
反応式
Cl[C:2]1[N:7]=[CH:6][C:5]2[O:8][C:9]3[C:14]([C@@:15]4([CH2:19][O:18][C:17]([NH2:20])=[N:16]4)[C:4]=2[CH:3]=1)=[CH:13][C:12](B1OC(C)(C)C(C)(C)O1)=[CH:11][CH:10]=3.P([O-])([O-])([O-])=O.[K+].[K+].[K+].[F:38][C:39]1[C:44](I)=[C:43]([F:46])[CH:42]=[CH:41][N:40]=1>O1CCOCC1.O.CCOC(C)=O.CC(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)C.CC(P(C(C)(C)C)C1C=CC(N(C)C)=CC=1)(C)C.Cl[Pd]Cl>[F:38][C:39]1[C:44]([C:12]2[CH:13]=[C:14]3[C@@:15]4([CH2:19][O:18][C:17]([NH2:20])=[N:16]4)[C:4]4[CH:3]=[C:2]([C:15]5[CH2:14][CH2:9][O:8][CH2:5][CH:4]=5)[N:7]=[CH:6][C:5]=4[O:8][C:9]3=[CH:10][CH:11]=2)=[C:43]([F:46])[CH:42]=[CH:41][N:40]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 100 °C
実験手順
A 20 mL glass microwave reaction vessel was charged with (S)-3-chloro-7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5′H-spiro[chromeno[2,3-c]pyridine-5,4′-oxazol]-2′-amine (0.251 g, 0.608 mmol), potassium phosphate (0.269 g, 1.266 mmol), 2,4-difluoro-3-iodopyridine (0.122 g, 0.506 mmol) and bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium (II) (0.036 g, 0.051 mmol) in dioxane (3.2 mL) and water (0.8 mL). The reaction mixture was heated at 100° C. for 30 min in microwave reactor. After cooling the rt the mixture was diluted with EtOAc and water. The aqueous layer was washed twice with saturated Na2CO3. The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude residue was purified by silica gel chromatography (2-10% MeOH—CH2Cl2) to provide the desired product as a brown residue.
後処理
- temperatureAfter cooling the rt the mixture
- washThe aqueous layer was washed twice with saturated Na2CO3
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
- customThe crude residue was purified by silica gel chromatography (2-10% MeOH—CH2Cl2)
出典と根拠
- ORDレコード
- ord-41255c7fc8d446d6a8c584bccf1d945d
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08883782B2
反応ノート
読み込み中…