Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
5-(4-Hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione → 5-(1-(4-Hydroxyphenyl)but-2-yn-1-yl)-2,2-dimethyl-1,3-dioxane-4,6-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 5-(4-Hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 370541 | — |
| 반응물 | Potassium bisulfate | HCID 516920 | — |
| 반응물 | HCID 178419101 | HCID 178419101 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ammonium Chloride | HCID 25517 | — |
| 생성물 | 5-(1-(4-Hydroxyphenyl)but-2-yn-1-yl)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 59855133 | 100% |
반응 단계
To a 250 mL 3-necked RB flask fitted with magnetic stirrer was charged with bromo(prop-1-yn-1-yl)magnesium (42.5 mL, 211 mmol) in THF (30 mL). To the RM was added slowly 5-(4-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5.0 g, 100.8 mmol) in THF (20 mL) under nitrogen atmosphere. The RM was stirred at room temperature about 30 minutes. The reaction mixture was diluted with NH4Cl solution and hexane. The aqueous layer was acidified with KHSO4 solution to adjust the pH 2 and extracted with ethyl acetate, washed with water, then dried to obtain the product (5.8 g, yield: 100.0%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09278915B2 |
| 출처 데이터셋 | uspto-grants-2016_03 |
| ORD ID | ord-b221ad47576d4438b29f562d6346b4b9 |
| 출처 메모 | uspto-grants-2016_03 |