Thiobenzamide → Methyl 2-phenyl-4,5,6,7-tetrahydrobenzo[d]thiazole-7-carboxylate
反応式
Br[CH:2]1[C:7](=O)[CH2:6][CH2:5][CH2:4][CH:3]1[C:9]([O:11][CH3:12])=[O:10].[C:13]([NH2:21])(=[S:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CCO>[C:14]1([C:13]2[S:20][C:2]3[CH:3]([C:9]([O:11][CH3:12])=[O:10])[CH2:4][CH2:5][CH2:6][C:7]=3[N:21]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1参加物
4
実験手順
A soln. of methyl 2-bromo-3-oxocyclohexanecarboxylate (100 mg, 0.43 mmol) and thiobenzamide (64 mg, 0.47 mmol) in EtOH (2 mL) was stirred at 85° C. overnight. Subsequently, the mixture was quenched with aq. sat. NaHCO3 and extracted with EtOAc. The comb. org. layers were washed with brine, dried over MgSO4, and conc. in vacuo. Purification by means of CC (2-15% EtOAc/Hept) provided a yellow oil.
後処理
- customSubsequently, the mixture was quenched with aq. sat. NaHCO3
- extractionextracted with EtOAc
- washlayers were washed with brine
- dry with materialdried over MgSO4
- customPurification by means of CC (2-15% EtOAc/Hept)
- customprovided a yellow oil
出典と根拠
- ORDレコード
- ord-6e769148e7034c299eae2b771e341106
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388197B2
反応ノート
読み込み中…