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 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Diethyl ((3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methyl)phosphonate | HCID 70421 | — |
반응 단계
20.63 g (100 mmol) of 2,6-di-tert-butylphenol, 5.22 g (174 mmol) of paraformaldehyde, 6.1 g (45 mmol) of 33% ethanolic dimethylamine and 26 ml (=24.7 g) of N,N-dimethylformamide are heated at 50° C. under nitrogen for 1 hour in a sulfonation flask fitted with a reflux condenser and mechanical stirrer. 33.23 g (200 mmol) of triethyl phosphite are added to this mixture. It is heated under reflux at a reaction temperature of 105° C.; the conversion to the final product is 82% (HPLC). Working-up: extraction (water/methylcyclohexane) and recrystallization (methylcyclohexane). Yield: 23.0 g (65%), melting point 120° C., purity (HPLC): 98%.
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-c78b3fa2db894452937fd0352cb9630a |
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| 출처 메모 | uspto-grants-1993_11 |
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