Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Boron trifluoride → HCID 14726544, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Boron trifluoride | HCID 6356 | — |
| 반응물 | N'-Hydroxy-4-methylbenzenecarboximidamide | HCID 209113 | — |
| 반응물 | 5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalene-2-carbonyl chloride | HCID 2795466 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 14726544 | HCID 14726544 | 30.8% |
반응 단계
8.0 g (30 millimoles) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthoyl chloride and 4.5 g (30 millimoles) of 4-methylbenzamidoxime in 250 ml of dioxane were refluxed for 1 hour. 1 ml of boron trifluoride dietherate were added and refluxing was continued for a further 4 hours. The mixture was allowed to cool, poured onto ice/water and extracted with methylene chloride. The organic phase was washed several times with water, dried over magnesium sulfate and evaporated down. The oily residue was purified by column chromatography (silica gel; n-heptane +0.5% of ethyl acetate), and the crude product obtained from the first fractions was recrystallized from methanol to give 3.2 g of the title compound of melting point 106°-109° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05061705 |
| 출처 데이터셋 | uspto-grants-1991_10 |
| ORD ID | ord-6e7318013dd442b58c22effb8ebd67c3 |
| 출처 메모 | uspto-grants-1991_10 |