HRID2367271

反应详情

EQUATION

反应方程式

HRID 2367271 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To 4-[2-amino-6-(2,3-dihydro-1H-inden-1-ylamino)-4-pyrimidinyl]-2-fluorobenzonitrile (500 mg, 1.45 mmol) in ethanol (2 mL) was added hydrazine monohydrate (3 mL, 74.0 mmol), and the reaction mixture was heated to 100° C. for 1 hour in a BiotageInitiator® microwave synthesizer. Upon cooling, the reaction mixture was concentrated in vacuum and purified by HPLC to afford the title compound (100 mg) as a brown solid. LC-MS (ES) m/z=358 [M+H]+. 1H NMR (400 MHz, DMSO-d6): δ 1.81 (s, 1H), 1.90-1.92 (m, 1H), 2.84-3.051 (m, 2H), 5.43 (s, 2H), 5.71 (s, 1H), 6.12 (s, 2H), 6.40 (s, 1H), 7.23-7.48 (m, 6H), 7.75 (d, J=8.4 Hz, 1H), 7.90 (s, 1H), 11.58 (s, 1H).

WORKUP

后处理

  1. temperatureUpon cooling
  2. concentrationthe reaction mixture was concentrated in vacuum
  3. custompurified by HPLC