Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → 2-Tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | 2,5-Dimethyl-2,5-hexanediol | HCID 8031 | — |
| 반응물 | Pivalaldehyde | HCID 12417 | — |
| 촉매 | p-Toluenesulfonic acid | HCID 6101 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane | HCID 13980748 | 85% |
반응 단계
A mixture of 730 g (5 mol) of 2,5-dimethylhexane-2,5-diol, 3 g of p-toluenesulfonic acid, 430 g (5 mol) of pivalaldehyde and 1 l of toluene was refluxed for 4 hours (h) during which the water of reaction produced (90 ml) was removed. The reaction mixture was then cooled down to room temperature (RT) and stirred up with 10 ml of 25% strength aqueous sodium hydroxide solution, the phases were separated, the organic phase was washed with a little water until neutral, and the toluene was then removed at 50°-60° C. The residue obtained was fractionated under reduced pressure affording 909 g (4.25 mol) of 2-tert.-butyl-4,4,7,7,-tetramethyl-1,3-dioxacycloheptane (boiling point 54° C./0.2 mbar). This corresponds to a yield of 85% of theory.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04707302 |
| 출처 데이터셋 | uspto-grants-1987_11 |
| ORD ID | ord-03ed008d92b34129a4600f2fd633702e |
| 출처 메모 | uspto-grants-1987_11 |