反応 #2257944

反応方程式

NaBH(OAc)3

solution

7-((R)-sec-Butoxy)-1-(4-chloro-phenyl)-2-{4-[(trans-4-ethylamino-cyclohexylmethyl)-methyl-amino]-phenyl}-6-methoxy-1,4-dihydro-2H-isoquinolin-3-one

AcOH

formaldehyde

→

title compound

収率 44.0%

7-((R)-sec-Butoxy)-1-(4-chloro-phenyl)-2-(4-{[4-(ethyl-methyl-amino)-trans-cyclohexylmethyl]-methyl-amino}-phenyl)-6-methoxy-1,4-dihydro-2H-isoquinolin-3-one

収率 44.0%

溶媒

MeCN

反応条件

後処理

1. 1
   その他at RT
2. 2
   その他then directly subjected to purification by reverse phase prep-HPLC (Waters system)

実験手順

To a solution of Example 52 (13.8 mg, 0.023 mmol) in MeCN (0.5 ml) were successively added AcOH (0.003 ml, 0.046 mmol), formaldehyde (37% in water, 0.003 ml, 0.046 mmol) and NaBH(OAc)3 (9.7 mg, 0.046 mmol) at RT. The reaction mixture was stirred at RT for 2 h then directly subjected to purification by reverse phase prep-HPLC (Waters system) to yield the title compound (TFA salt, 7.4 mg, 0.010 mmol, 44%) as a colorless solid. HPLC: AtRet=2.01 min; LC-MS: m/z 618.4 [M+H]+.

出典