Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trimethylolpropane → 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trimethylolpropane | HCID 6510 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,1-Dimethoxyethane | HCID 10795 | — |
| 촉매 | Diammonium molybdate | HCID 61578 | — |
| 촉매 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1,3-Dioxane-5-methanol, 5-ethyl-2,2-dimethyl- | HCID 11816152 | 95% |
반응 단계
Trimethylolpropane (10.0 g; 74.6 mmol), 2,2-dimethoxyethane (9.01 g; 86.5 mmol) and p-toluenesulfonic acid monohydrate (0.369 g; 1.94 mmol) were dissolved in tetrahydrofuran (125 mL). The clear solution was stirred at ambient temperature for 24 h. TLC (stained with ammonium molybdate) confirmed near quantitative conversion of the starting triol. The reaction was neutralised with triethylamine (10 mL) and all volatiles were removed in vacuo. Colourless oily residue was passed through a silicagel column (eluent ethyl acetate/cyclohexane 1:1). The eluent was evaporated to provide (5-ethyl-2,2-dimethyl-1,3-dioxan-5-yl)methanol (12.34 g; 95% yield) as a colourless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09296835B2 |
| 출처 데이터셋 | uspto-grants-2016_03 |
| ORD ID | ord-36b3516933c442f9b5823fb96a670468 |
| 출처 메모 | uspto-grants-2016_03 |