Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium hydroxide monohydrate → 4-Hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium hydroxide monohydrate | HCID 23719240 | — |
| 반응물 | HCID 86615847 | HCID 86615847 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | 4-Hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid | HCID 22708342 | — |
반응 단계
A solution of 4-hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid, methyl ester in iso-propanol (50 mL) was added to KOH/H2O (20%, 60 mL) and the mixture was refluxed overnight. The resultant solution was partially concentrated, and the remainder was acidified with H2SO4 (10%). The very turbid mixture was extracted with ether (3×), and the combined organic phase was dried (Na2SO4) and concentrated. The crude product was purified via prep-HPLC (CH3CN:0.1M ammonium acetate (30:60)). The fractions of interest were partly concentrated and extracted with ether. The combined organic layers were washed with water, dried (Na2SO4), and concentrated, yielding 0.24 g (10% over steps (vi)–(ix)).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07241757B2 |
| 출처 데이터셋 | uspto-grants-2007_07 |
| ORD ID | ord-3791df1d48984dd887b850861a79aae0 |
| 출처 메모 | uspto-grants-2007_07 |