Hydrochloric Acid → HCID 118061513, compound

HRID 575526Notes

Reaction equation

HRID 575526 reaction equation
[NH2:1][C:2]1[C:7]([CH2:8][CH2:9][CH:10]2[CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11]2)=[C:6]([Cl:23])[N:5]=[C:4]([CH3:24])[N:3]=1.Cl>O1CCOCC1>[ClH:23].[Cl:23][C:6]1[N:5]=[C:4]([CH3:24])[N:3]=[C:2]([NH2:1])[C:7]=1[CH2:8][CH2:9][CH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 118061152HCID 118061152, compound

Product 1

HCID 118061513HCID 118061513, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

Dissolve tert-butyl 4-[2-(4-amino-6-chloro-2-methyl-pyrimidin-5-yl)ethyl]piperidine-1-carboxylate (29.00 g, 81.72 mmol) in 1,4-dioxane (145 mL) and add 4M hydrogen chloride in 1,4-dioxane (204.2 mL, 817.1 mmol). Stir the solution for 18 h at RT. Concentrate the mixture under reduced pressure, slurry in diethyl ether (250 mL), filter, and dry the resultant solid under vacuum to give the title compound as a crude white solid (29 g). LC-ES/MS m/z (35Cl/37Cl) 255.2/257.2 (M+1).

Workup

  1. concentrationConcentrate the mixture under reduced pressure, slurry in diethyl ether (250 mL)
  2. filtrationfilter
  3. customdry the resultant solid under vacuum

Sources & evidence

ORD record
ord-8c6e04c98a5844e18c54a918a8b572d0
Source dataset
uspto-grants-2015_05
Patent number
US09035051B1

Reaction notes

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