HRID1695935

反应详情

EQUATION

反应方程式

HRID 1695935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(2-(2-(dimethylamino)ethylamino)-3-fluorophenyl)methanol (536 mg, 2.525 mmol) and MnO2 (878.1 mg, 174.7 μL, 10.10 mmol) were heated to reflux in toluene (13 mL) overnight. The suspension was filtered through Celite with CH2Cl2 and concentrated on a rotary evaporator. The crude product was purified on 12 g Redisep ISCO column eluting with 4-55% EtOAc/Hexanes over 30 CV. 2-(2-(Dimethylamino)ethylamino)-3-fluorobenzaldehyde was identified by 1H-NMR and carried on to next reaction.

WORKUP

后处理

  1. filtrationThe suspension was filtered through Celite with CH2Cl2
  2. concentrationconcentrated on a rotary evaporator
  3. customThe crude product was purified on 12 g Redisep ISCO column
  4. washeluting with 4-55% EtOAc/Hexanes over 30 CV
  5. customcarried on to next reaction