Sulfuric Acid → HCID 20275489, compound

HRID 370756Notes

Reaction equation

HRID 370756 reaction equation
[CH3:1][C:2]1([CH3:11])[NH:8][C:7]([CH3:10])([CH3:9])[CH2:6][C:4](=O)[CH2:3]1.[NH2:12][CH2:13][CH2:14][NH:15][CH2:16][CH2:17][NH2:18].S(=O)(=O)(O)O>CO.[Pd]>[CH3:1][C:2]1([CH3:11])[CH2:3][CH:4]([NH:12][CH2:13][CH2:14][NH:15][CH2:16][CH2:17][NH2:18])[CH2:6][C:7]([CH3:10])([CH3:9])[NH:8]1

Participants

6

Reactant 3

HCID 1118Sulfuric AcidHCID 8111DiethylenetriamineHCID 132202,2,6,6-Tetramethyl-4-piperidone

Product 1

HCID 20275489HCID 20275489, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

A mixture of 155 g of triacetone amine, 113 g of diethylene triamine, and 2.5 g of conc. sulfuric acid in 2.5 liters of methanol is hydrogenated in the presence of 7 g of 5% palladium on carbon in the manner described in Example 1. In addition to yielding 1,7-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,4,7-triazaheptane, distillation of the hydrogenation mixture yields at 115°-118° C./0.09 mm Hg 1-(2,2,6,6-tetramethyl-4-piperidyl)-1,4,7-triazaheptane as main product.

Workup

  1. additionIn addition
  2. customto yielding
  3. distillation1,7-bis(2,2,6,6-tetramethyl-4-piperidyl)-1,4,7-triazaheptane, distillation of the hydrogenation mixture

Sources & evidence

ORD record
ord-f6e4be2614a74b2c9d74feecd541f3d8
Source dataset
uspto-grants-1985_07
Patent number
US04528374

Reaction notes

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