Hydrochloric Acid → HCID 58193747、化合物
反応式
[NH2:1][CH2:2][CH2:3][NH:4][C:5]([C:7]1([C:11]#[N:12])[CH2:10][CH2:9][CH2:8]1)=O.C1COCC1.B.C1COCC1.Cl>O.C(O)C.CC(C)=O>[NH2:12][CH2:11][C:7]1([CH2:5][NH:4][CH2:3][CH2:2][NH2:1])[CH2:10][CH2:9][CH2:8]1[NH2:1][CH2:2][CH2:3][NH:4][C:5]([C:7]1([C:11]#[N:12])[CH2:10][CH2:9][CH2:8]1)=O.C1COCC1.B.C1COCC1.Cl>O.C(O)C.CC(C)=O>[NH2:12][CH2:11][C:7]1([CH2:5][NH:4][CH2:3][CH2:2][NH2:1])[CH2:10][CH2:9][CH2:8]1
6.37 g (0.038 mol) of 5 and 50 mL of anhydrous THF were mixed, followed by adding 300 mL of 1 M BH3-THF solution to the mixture in an ice bath (−10° C.) of liquid nitrogen and acetone under a nitrogen gas environment to form a reaction solution. The reaction solution was subjected to reaction at −5˜0° C. for 1 hour, followed by heating the reaction solution to 70° C. to allow reaction to take place for 36 hours, and evaporating to obtain a solid substance. The solid substance, 100 mL of ethanol and 10 mL of 6N HCl were mixed, refluxed for 12 hours, followed by evaporation to form yellow oil. The yellow oil was stirred in water and was mixed with HCl to adjust pH to 2 to obtain a crude product. The crude product was purified by placing in a column (3×20 cm) filled with 100 mL of AG 50 W×8 cationic exchange resin and elutriating HCl solutions having gradient concentrations, collecting an eluent fraction of gradient concentration from 3.5 N to 4.0 N, and followed by evaporating the eluent fraction to obtain 2.98 g (0.019 mol, 50%) of 6.
読み込み中…
