Hydrochloric Acid → HCID 66701244, compound

HRID 1517365Notes

Reaction equation

HRID 1517365 reaction equation
[ClH:1].[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>[ClH:1].[ClH:1].[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

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 out by addition of acetone, and finally diethyl ether was added and the precipitate formed was filtered off 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 out by addition of acetone, and finally diethyl ether
  5. additionwas added
  6. customthe precipitate formed
  7. filtrationwas filtered off with suction

Sources & evidence

ORD record
ord-81273a3d03034c8784d36cbd45700a1a
Source dataset
uspto-grants-2012_07
Patent number
US08232288B2

Reaction notes

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