1,3,2-Dioxaphosphorinane, 2-chloro-5,5-dimethyl- → HCID 21277936, compound
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
Reactant 2
Product 1
Reagents, catalysts & solvents 2
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
- temperatureAfter heating at the reflux temperature for 15 hours
- filtrationthe precipitated hydrochloride is filtered off
- 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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