Reaction equation
[CH3:1]C1C(C)=NC(C)(C)CN=1.C=O.[C:13]([C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([CH3:26])([CH3:25])[CH3:24])[C:18]=1[OH:27])([CH3:16])([CH3:15])[CH3:14].CNC.[P:31]([O:38]CC)([O:35][CH2:36][CH3:37])[O:32][CH2:33][CH3:34]>>[C:23]([C:19]1[CH:20]=[C:21]([CH:22]=[C:17]([C:13]([CH3:16])([CH3:15])[CH3:14])[C:18]=1[OH:27])[CH2:1][P:31](=[O:38])([O:35][CH2:36][CH3:37])[O:32][CH2:33][CH3:34])([CH3:26])([CH3:25])[CH3:24]Participants
Conditions
- Temperature
- 85 °C
Procedure
3.2 g of HTMP (hydroxymethylpiperidine), 52.3 g of paraformaldehyde and 206.3 g of 2,6-di-tert-butylphenol are rendered inert and are initially introduced at 60° C. under reduced pressure into a double-jacketed flask with an outlet at the bottom, a baffle, an impeller stirrer and a sublevel air lock for gas introduction. 52 g of dimethylamine gas are introduced at this temperature and the mixture is stirred at 85° C. for 1 hour. Addition of 332 g of triethyl phosphite is then carried out, after which the reaction mixture is kept at 115° C. for 4 hours. Working-up: distillation of triethyl phosphite and dimethylamine under reduced pressure and crystallization of the residue from ligroin yield 320 g of product (90%), melting point 114° C.
Workup
- additionare initially introduced at 60° C. under reduced pressure into a double-jacketed flask with an outlet at the bottom, a baffle, an impeller stirrer
- waitafter which the reaction mixture is kept at 115° C. for 4 hours
- distillationWorking-up: distillation of triethyl phosphite and dimethylamine
- customunder reduced pressure and crystallization of the residue from ligroin yield 320 g of product (90%), melting point 114° C.
Sources & evidence
- ORD record
- ord-6e451c96394449579e8b8010653c5b12
- Source dataset
- uspto-grants-1993_11
- Patent number
- US05258540
Linked notes
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