Phosgene → HCID 10866933, compound

HRID 1184342Notes

Reaction equation

HRID 1184342 reaction equation
O=C(Cl)[O:3][C:4]([Cl:7])(Cl)Cl.[C:9]([Cl:12])(Cl)=O.[NH:13]1C[CH2:17][CH2:16][CH2:15][C:14]1=O>C(OCC)(=O)C>[Cl:12][C:9]1[N:13]([C:4]([Cl:7])=[O:3])[CH2:14][CH2:15][CH2:16][CH:17]=1

Participants

5

Reactant 3

HCID 6371PhosgeneHCID 10426DiphosgeneHCID 126652-Piperidone

Product 1

HCID 10866933HCID 10866933, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To stirred diphosgene (3.10 ml, 25.7 mmol) at ˜−20° C. (cooled with a dry ice/2-propanol bath) under nitrogen was added activated carbon (0.25 g), which caused some phosgene gas to be liberated. To the resulting stirred mixture was added very slowly dropwise piperidin-2-one (2.55 g, 25.7 mmol) in ethyl acetate (dried over molecular sieves) (7 ml) over 1 hour, while keeping the temperature below 0° C.

Workup

  1. temperature(cooled with a dry ice/2-propanol bath) under nitrogen
  2. additionwas added activated carbon (0.25 g), which
  3. customthe temperature below 0° C.

Sources & evidence

ORD record
ord-459b24b65211463da40407e718de1fe4
Source dataset
uspto-grants-2014_03
Patent number
US08669208B2

Reaction notes

Loading…