反応 #2257956

反応方程式

mixture

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

formaldehyde

→

title compound

収率 98.0%

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

収率 98.0%

溶媒

2-propanol

反応条件

後処理

1. 1
   濃縮The mixture was concentrated to dryness
2. 2
   その他the residue was purified by reversed phase column chromatography
3. 3
   workup.ADDITIONThe fractions containing the product
4. 4
   workup.ADDITION(addition of NaHCO3)

実験手順

The mixture of Example 131 (80 mg, 0.121 mmol) and formaldehyde (0.090 mL, 37% solution, 10 eq., 1.208 mmol) was heated for 5 h in 2-propanol (4 mL) at 85° C. The mixture was concentrated to dryness and the residue was purified by reversed phase column chromatography. The fractions containing the product were pooled and worked up (addition of NaHCO3), yielding the title compound as an off-white solid (46 mg, 0.068 mmol, >98%). HPLC: HtRet=1.40 min; LC-MS: m/z 674.2 [M+H]+.

出典