1,3,2-Dioxaphosphorinane, 2-chloro-5,5-dimethyl- → HCID 21277936, compound

HRID 2291815Notes

Reaction equation

HRID 2291815 reaction equation
Cl[P:2]1[O:7][CH2:6][C:5]([CH3:9])([CH3:8])[CH2:4][O:3]1.[CH2:10]([NH:14][CH:15]1[CH2:20][C:19]([CH3:22])([CH3:21])[N:18]([CH3:23])[C:17]([CH3:25])([CH3:24])[CH2:16]1)[CH2:11][CH2:12][CH3:13]>C(N(CC)CC)C.C1(C)C=CC=CC=1>[CH2:10]([N:14]([CH:15]1[CH2:16][C:17]([CH3:25])([CH3:24])[N:18]([CH3:23])[C:19]([CH3:21])([CH3:22])[CH2:20]1)[P:2]1[O:7][CH2:6][C:5]([CH3:9])([CH3:8])[CH2:4][O:3]1)[CH2:11][CH2:12][CH3:13]

Participants

5

Procedure

18.4 g of 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane are added dropwise, at room temperature, with stirring, to a solution of 19.7 g (0.1 mol) of 4-butylamino-1,2,2,6,6-pentamethylpiperidine in 100 ml of triethylamine. After heating at the reflux temperature for 15 hours, the mixture is diluted with toluene and the precipitated hydrochloride is filtered off. Evaporation of the filtrate gives 2-[N-butyl(1,2,2,6,6-pentamethyl-4-piperidyl)amino]-5,5-dimethyl-1,3,2-dioxaphosphorinane as an oil which boils at 120° under 40 Pa (Compound No. 1).

Workup

  1. temperatureAfter heating at the reflux temperature for 15 hours
  2. filtrationthe precipitated hydrochloride is filtered off
  3. customEvaporation of the filtrate

Sources & evidence

ORD record
ord-c81b25b3d8ba436cb0ab76aa8d8515ec
Source dataset
uspto-grants-1989_01
Patent number
US04798822

Reaction notes

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