HRID469101

反应详情

EQUATION

反应方程式

HRID 469101 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared according to general procedure AT using methyl 5-({[(4-methoxy-2,6-dimethylphenyl)sulfonyl](methyl)amino}methyl)-1,3,4-oxadiazole-2-carboxylate (30 mg, 0.08 mmol), 1-{4-[(3-methoxypyrrolidin-1-yl)methyl]phenyl}-N-methylmethanamine (45 mg, 0.19 mmol) and trimethylaluminium (2 M in toluene, 0.08 mL) in DCE (5 mL). The crude product was purified using FCC, eluting with 95:4.5:0.5 DCM:MeOH:NH3. The fraction collected was dissolved in DCM (5 mL) and shaken with PL-MIA resin for 2 h, and the beads were filtered and washed with DCM (10 mL). The combined filtrates were concentrated in vacuo and the residue purified using prep method D to afford the title compound.

WORKUP

后处理

  1. customThe title compound was prepared
  2. customThe crude product was purified
  3. washeluting with 95:4.5:0.5 DCM
  4. customThe fraction collected
  5. dissolutionwas dissolved in DCM (5 mL)
  6. filtrationthe beads were filtered
  7. washwashed with DCM (10 mL)
  8. concentrationThe combined filtrates were concentrated in vacuo
  9. customthe residue purified