HRID880830

反应详情

EQUATION

反应方程式

HRID 880830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 50 mg of 2-chloro-N-(6-oxo-5,6-dihydro-phenanthridin-2-yl)acetamide (XV) (0.17 mmol) in N,N-dimethylformamide (3 mL), 0.09 mL of (3-amino-propyl)-carbamic acid tert-butyl ester (0.51 mmol) and 0.036 mL of triethylamine (0.26 mmol) were added. The reaction mixture was stirred at room temperature overnight, evaporated to dryness and then purified through preparative HPLC on a Waters X Terra RP 18 (19×250 mm, 5 □m) column. Mobile phase A was 0.05% ammonia/acetonitrile:95/5 and mobile phase B was acetonitrile/water:95/5. Gradient from 10 to 75% B in 15 min. Fractions containing the desired compound were dried, affording 32 mg (44% yield) of the title compound.

WORKUP

后处理

  1. additionwere added
  2. customevaporated to dryness
  3. custompurified through preparative HPLC on a Waters X Terra RP 18 (19×250 mm, 5 □m) column
  4. waitGradient from 10 to 75% B in 15 min
  5. additionFractions containing the desired compound
  6. customwere dried