Hydrogen Peroxide → HCID 87152024, compound

HRID 1531607Notes

Reaction equation

[CH3:1][C:2]1([CH3:32])[CH2:7][CH:6]([N:8]([CH:28]=[O:29])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][N:15]([CH:18]2[CH2:23][C:22]([CH3:25])([CH3:24])[NH:21][C:20]([CH3:27])([CH3:26])[CH2:19]2)[CH:16]=[O:17])[CH2:5][C:4]([CH3:31])([CH3:30])[NH:3]1.[O-:33]S([O-])(=O)=O.[Mg+2].OO.[OH-:41].[K+]>CO>[OH:41][N:21]1[C:22]([CH3:24])([CH3:25])[CH2:23][CH:18]([N:15]([CH:16]=[O:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][N:8]([CH:6]2[CH2:5][C:4]([CH3:31])([CH3:30])[N:3]([OH:33])[C:2]([CH3:32])([CH3:1])[CH2:7]2)[CH:28]=[O:29])[CH2:19][C:20]1([CH3:27])[CH3:26]

Participants

Conditions

Temperature: 81 °C

Procedure

A solution of 337.5 g (0.75 mol) of N,N′-bis-[2,2,6,6-tetra-methylpiperidin-4-yl]-N,N′-bisformyl-1,6-diaminohexane in 600 ml of methanol was treated with 0.15 g of MgSO4. 600 ml of a 30% strength H2O2 solution (5.87 mol) were added dropwise at 67° C. in the course of 6 h. The temperature was then increased to 81° C. and the mixture was kept at this temperature for a further 6 h, the pH of 7.8 being kept constant by metered addition of a 50% strength KOH solution. The pH was then adjusted to 9.0 by addition of KOH solution. After the mixture had been left at this pH for a further 2 h, the methanol was distilled off, the product being precipitated. It was washed with water and dried.

Workup

waitAfter the mixture had been left at this pH for a further 2 h
distillationthe methanol was distilled off
customthe product being precipitated
washIt was washed with water
customdried

Sources & evidence

ORD record: ord-4f22144f22894a99ab2aac87b63f4af4
Source dataset: uspto-grants-2001_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06200460B1

Reaction notes

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