Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3,4-dihydro-2H-pyran → 2-(3-Iodo-benzyloxy)-tetrahydro-pyran
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 반응물 | 3-Iodobenzyl alcohol | HCID 42300 | — |
| 촉매 | p-Toluenesulfonic acid | HCID 6101 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(3-Iodo-benzyloxy)-tetrahydro-pyran | HCID 60133698 | 103.6% |
반응 단계
para-Toluenesulfonic acid (100 mg, cat.) was added in one portion to a cooled solution (0 C) of 3-iodobenzyl alcohol (4.71 g, 0.02 mol) and dihydropyran (1.86 g, 0.022 mol) in dichloromethane (50 mL) under a nitrogen atmosphere. The cooling bath was removed and the reaction mixture was allowed to warm to room temperature over 1 hr. Diethyl ether (100 mL) was then added followed by saturated sodium hydrogen carbonate solution (100 mL). The organic layer was separated, dried (MgSO4) and evaporated in vacuo to yield the crude product (6.59 g) A332.1, which was used immediately without further purification. HPLC YMC S-5 4.6×33 mm (2 min grad): retention time 2.16 min, no M+H+ observed.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737279B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-13b29cc03d364b6f9c3b6efe538009bf |
| 출처 메모 | uspto-grants-2010_06 |