Trifluoroacetic acid → HCID 23079692, compound

HRID 2112759Notes

Reaction equation

HRID 2112759 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][O:5][CH:4]([CH2:8][N:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]2)[CH2:3]1.FC(F)(F)C(O)=O>ClCCl>[CH3:1][N:2]1[CH2:7][CH2:6][O:5][CH:4]([CH2:8][N:9]2[CH2:10][CH2:11][NH:12][CH2:13][CH2:14]2)[CH2:3]1

Participants

4

Procedure

Tert-butyl 4-(4-methylmorpholin-2-ylmethyl)piperazine-1-carboxylate (5.00 g, 17.0 mmol) prepared according to Process Step 2 was dissolved in dichloromethane (60 mL), and the solution was mixed with trifluoroacetic acid (20 mL) added dropwise under ice-cooling. After stirring at room temperature for one hour, the solvent was distilled off under reduced pressure. The resulting yellow oil was dissolved in dioxane (100 mL), and the solution was mixed with triethylamine (20 mL) to thereby yield 4-methyl-2-piperazin-1-ylmethylmorpholine.

Workup

  1. additionadded dropwise under ice-
  2. temperaturecooling
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionThe resulting yellow oil was dissolved in dioxane (100 mL)
  5. additionthe solution was mixed with triethylamine (20 mL) to thereby yield 4-methyl-2-piperazin-1-ylmethylmorpholine

Sources & evidence

ORD record
ord-4d42e23ecfe84eb1ac372dc1e8f9c1d8
Source dataset
uspto-grants-2009_04
Patent number
US07524852B2

Reaction notes

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