HRID130687

反应详情

EQUATION

反应方程式

HRID 130687 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add benzaldehyde (7.5 mL, 74 mmol) to a stirred solution of tyramine (10.00 g, 73 mmol) and anhydrous methanol (90 mL). Bleat reaction to reflux for 1 h under nitrogen. Cool reaction to 0° C. and slowly add sodium borohydride (2.84 g, 75 mmol). Stir for 1 h at room temperature and then concentrate on a rotary evaporator. Add water (100 mL) and stir for 1.5 h at room temperature. Filter and wash with water to yield 10.11 g (61%) of 4-(2-benzylamino-ethyl)-phenol: mass spectrum (ion spray): m/z=228.1 (M+1); 1H NMR (DMSO-d6): 9.14 (br s, 1H), 7.29-7.18 (m, 5H), 6.96 (d, 2H), 6.65 (d, 2H), 3.69 (s, 2H), 2.67-2.60 (m, 4H), 2.02 (br s, 1H).

WORKUP

后处理

  1. customBleat reaction
  2. temperatureto reflux for 1 h under nitrogen
  3. temperatureCool
  4. customreaction to 0° C.
  5. concentrationconcentrate on a rotary evaporator
  6. stirringAdd water (100 mL) and stir for 1.5 h at room temperature
  7. filtrationFilter
  8. washwash with water