참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | Formaldehyde | HCID 712 | — |
| 반응물 | Triethyl phosphite | HCID 31215 | — |
| 반응물 | 2,6-Di-tert-butylphenol | HCID 31405 | — |
| 반응물 | 3-Hydro-2,2,5,6-tetramethylpyrazine | HCID 10261158 | — |
| 생성물 | Diethyl ((3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methyl)phosphonate | HCID 70421 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05258540 |
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| 출처 데이터셋 | uspto-grants-1993_11 |
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| ORD ID | ord-6e451c96394449579e8b8010653c5b12 |
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| 출처 메모 | uspto-grants-1993_11 |
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