HRID1405366

反应详情

EQUATION

反应方程式

HRID 1405366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 2-methyl-6,7-bis(trifluoromethyl)spiro[3,4-dihydropyrrolo[1,2-a]pyrazine-1,4′-piperidine]-1′-carboxylate (from step 1) was taken up in CH2Cl2 (2 mL) and HCl (1.7 mL of 4 M, 6.8 mmol) was added. The mixture was allowed to stir for 30 min before it was concentrated under reduced pressure. The residue was taken up in ethyl acetate and was washed with sat. aq. NaHCO3, then brine. The organic layer was dried over sodium sulfate, filtered and concentrated to give 2-methyl-6,7-bis(trifluoromethyl)spiro[3,4-dihydropyrrolo[1,2-a]pyrazine-1,4′-piperidine] (22 mg, 2% over 2 steps). ESI-MS m/z calc. 341.1, found 342.3 (M+1)+; Retention time: 1.29 minutes.

WORKUP

后处理

  1. concentrationwas concentrated under reduced pressure
  2. washwas washed with sat. aq. NaHCO3
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated