Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Chloride → 3-(4-Hydroxyphenyl)hex-4-ynoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | Ethyl ketone | HCID 7288 | — |
| 반응물 | 5-(1-(4-Hydroxyphenyl)but-2-yn-1-yl)-2,2-dimethyl-1,3-dioxane-4,6-dione | HCID 59855133 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-(4-Hydroxyphenyl)hex-4-ynoic acid | HCID 59855136 | 77.5% |
반응 단계
A 1L RB flask was charged with compound 1.2 (37 g), diethyl ketone (160 mL), and water (80 mL). The suspension was heated to reflux for 48 h. After cooling, the aqueous layer was saturated with NaCl(s) and separated. The organic layer was dried over MgSO4, filtered, and concentrated to a light brown oil which was crystallized from hot ethyl acetate:hexanes (1:2). After collecting and drying, the product was obtained as an off-white powder (20.3 g, 77%). 1H NMR(500 MHz)(DMSO-d6) δ 12.2 (s, 1H); 9.27 (s, 1H); 7.12 (d, 2H, J=8.5 Hz); 6.67 (d, 2H, J=8.6 Hz); 3.87 (m, 1H); 2.54 (m, 2H); 1.82 (d, 3H, J=2.4 Hz). MS ESI (pos.) m/e: 205.1 (M+H); 227.1 (M+Na).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07816367B2 |
| 출처 데이터셋 | uspto-grants-2010_10 |
| ORD ID | ord-8ea5cea0fab04f41b2ec230158506c04 |
| 출처 메모 | uspto-grants-2010_10 |