反応 #2179577

反応方程式

mixture

2-{4-[({6-[(S)-1-(4-Chloro-phenyl)-7-isopropoxy-6-methoxy-3-oxo-3,4-dihydro-1H-isoquinolin-2-yl]-pyridin-3-yl}-methyl-amino)-methyl]-trans-cyclohexylamino}-N-methyl-acetamide

formaldehyde

→

title compound

収率 79.0%

(S)-1-(4-Chloro-phenyl)-7-isopropoxy-6-methoxy-2-(5-{methyl-[4-(3-methyl-4-oxo-imidazolidin-1-yl)-trans-cyclohexylmethyl]-amino}-pyridin-2-yl)-1,4-dihydro-2H-isoquinolin-3-one

収率 79.0%

溶媒

EtOH

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated to dryness
2. 2
   その他the residue was purified by Combi-Flash Companion™ (Isco Inc.) column chromatography (SiO2; gradient elution, DCM/[DCM/MeOH 9: 1] 1:0→0:1)

実験手順

The mixture of Example 122 (38 mg, 0.061 mmol) and formaldehyde (0.046 ml, 37% solution, 10 eq, 0.612 mmol) was heated for 15 h in EtOH (1 mL) at 80° C. The reaction mixture was concentrated to dryness and the residue was purified by Combi-Flash Companion™ (Isco Inc.) column chromatography (SiO2; gradient elution, DCM/[DCM/MeOH 9: 1] 1:0→0:1) yielding the title compound as a colorless solid (31 mg, 0.048 mmol, 79%). HPLC: FtRet=1.236; LC-MS: m/z 646.4 [M+H]+.

出典