Acetone → 4-Piperidinone, 2,2,6,6-tetramethyl-, monohydrate

HRID 1657446

Reaction equation

HRID 1657446 reaction equation
[OH2:1].[CH3:2][C:3]1([CH3:12])[NH:8][C:7]([CH3:10])([CH3:9])[CH2:6][C:5]([CH3:11])=N1.CC(C)=[O:15]>CO>[OH2:15].[CH3:2][C:3]1([CH3:12])[CH2:11][C:5](=[O:1])[CH2:6][C:7]([CH3:10])([CH3:9])[NH:8]1

Participants

4

Reactant 2

HCID 180AcetoneHCID 180002252,2,4,4,6-Pentamethyl-2,3,4,5-tetrahydropyrimidine hydrate

Product 1

HCID 223976024-Piperidinone, 2,2,6,6-tetramethyl-, monohydrate

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 250 g of 2,2,4,4,6-pentamethyl-2,3,4,5-tetrahydropyrimidine hydrate, 100 g of acetone and 100 g of methanol is refluxed for 13 hours. The solution is subsequently concentrated in vacuo, and the oil remaining is distilled in vacuo. The yield is 185 g of a slightly yellowish oil, B.P.12 = 80°- 86°C, which, after the addition of about 22 ml of water, solidifies to form crystals of 2,2,6,6-tetramethyl-4-oxopiperidine-hydrate.

Workup

  1. temperatureis refluxed for 13 hours
  2. concentrationThe solution is subsequently concentrated in vacuo
  3. distillationthe oil remaining is distilled in vacuo
  4. additionThe yield is 185 g of a slightly yellowish oil, B.P.12 = 80°- 86°C, which, after the addition of about 22 ml of water

Sources & evidence

ORD record
ord-63b4b276e1bd4c39903a6e7159b8d402
Source dataset
uspto-grants-1976_06
Patent number
US03960875

Linked notes

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