Hydrochloric Acid → HCID 59401726, compound

HRID 1808360Notes

Reaction equation

HRID 1808360 reaction equation
Cl.[N:2]1([CH:6]2[CH2:23][CH2:22][C:9]3([CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]3)[CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3]1>CO>[N:2]1([CH:6]2[CH2:7][CH2:8][C:9]3([CH2:14][CH2:13][NH:12][CH2:11][CH2:10]3)[CH2:22][CH2:23]2)[CH2:3][CH2:4][CH2:5]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 66850495HCID 66850495, compound

Product 1

HCID 59401726HCID 59401726, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Hydrogen chloride in methanol (1.25 mol/l, 15.5 ml) was added to tert-butyl 9-(azetidin-1-yl)-3-azaspiro[5.5]undecane-3-carboxylate (1 g, 3.24 mmol), and the mixture was refluxed for 45 min. The solvent was removed in vacuo and the residue was dissolved in a small amount of ethanol. A solid was then precipitated by addition of acetone, and finally diethyl ether was added and the resulting precipitate was filtered out with suction. Yield: 0.87 g (95%)

Workup

  1. temperaturethe mixture was refluxed for 45 min
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in a small amount of ethanol
  4. customA solid was then precipitated by addition of acetone, and finally diethyl ether
  5. additionwas added
  6. filtrationthe resulting precipitate was filtered out with suction

Sources & evidence

ORD record
ord-13bd39f68d4b4c91aa7a8cff28e1973e
Source dataset
uspto-grants-2013_01
Patent number
US08357717B2

Reaction notes

Loading…