Dimethylamine → Diethyl ((3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methyl)phosphonate

HRID 466776

反応式

HRID 466776 の反応式
[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]

参加物

6

反応物 5

HCID 674DimethylamineHCID 712FormaldehydeHCID 31215Triethyl phosphiteHCID 314052,6-Di-tert-butylphenolHCID 102611583-Hydro-2,2,5,6-tetramethylpyrazine

生成物 1

HCID 70421Diethyl ((3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methyl)phosphonate

反応条件

温度
85 °C

実験手順

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.

後処理

  1. 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
  2. waitafter which the reaction mixture is kept at 115° C. for 4 hours
  3. distillationWorking-up:distillation of triethyl phosphite and dimethylamine
  4. customunder reduced pressure and crystallization of the residue from ligroin yield 320 g of product (90%), melting point 114° C.

出典と根拠

ORDレコード
ord-867b9c49a07a413eadd622bc41a08f46
出典データセット
uspto-grants-1992_10
特許番号
US05157141

関連ノート

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