Ethyl 2-bromopropionate → HCID 13909862、化合物

反応式

[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]2[N:17]3[N:12]([CH2:13][CH2:14][CH2:15][CH2:16]3)[C:11](=[O:18])[S:10]2)=[CH:4][C:3]=1[NH2:19].Br[CH:21]([CH3:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23].C(=O)([O-])O.[Na+]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]2[N:17]3[N:12]([CH2:13][CH2:14][CH2:15][CH2:16]3)[C:11](=[O:18])[S:10]2)=[CH:4][C:3]=1[NH:19][CH:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH3:27]

参加物

反応物 3

HCID 79040Ethyl 2-bromopropionate

HCID 516892Sodium Bicarbonate

HCID 19987017HCID 19987017、化合物

生成物 1

HCID 13909862HCID 13909862、化合物収率 52%

実験手順

Into a reaction flask equipped with a Dimroth condenser, 2.2 g (7.4 mmol) of 9-(4-chloro-3-aminophenylimino)-8-thia-1,6-diazabicyclo[4.3.0]nonane-7-one, 15 ml of ethyl 2-bromopropionate and 2.0 g (24 mmol) of sodium hydrogen carbonate, were charged, and refluxed under heating for 4 hours to complete the reaction. The reaction solution was filtered, concentrated and extracted with ethyl acetate, and then washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain a crude product, which was purified by column chromatography to obtain 1.5 g (yield: 52%) of colorless oily substance. Refractive index: nD20 1.5755