Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2,5-Bis-(methoxycarbonyl)-3-fur-3-yl-4-hydroxythiophene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 1,1'-Dimethyl 2,2'-thiobis(acetate) | HCID 85233 | — |
| 반응물 | Butyl 2-(fur-3-yl)-2-oxo-acetate | HCID 13986137 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2,5-Bis-(methoxycarbonyl)-3-fur-3-yl-4-hydroxythiophene | HCID 54708884 | — |
반응 단계
A mixture of 26 g of dimethyl thiodiacetate and 32 g of butyl 2-(fur-3-yl)-2-oxo-acetate is added dropwise, over 30 minutes at 64°-68° C., to a mixture of 100 ml of methyl alcohol and 39.9 g of potassium tert.-butanolate. The reaction mixture is kept at this temperature for a further 3 hours, and then poured into a mixture of 179 g of ice and 58 g of concentrated hydrochloric acid. The resultant crystals are separated off, washed with ice water until free of chloride, and dried at 60 C./0.1 mbar. Yield: 27.9 g. The product is recrystallized from 250 ml of methyl alcohol, and 22 g of 2,5-bis-(methoxycarbonyl)-3-fur-3-yl-4-hydroxythiophene having a melting point of 102° C. are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04757085 |
| 출처 데이터셋 | uspto-grants-1988_07 |
| ORD ID | ord-293b6a6f33014e599fc2bfa908b8f6f3 |
| 출처 메모 | uspto-grants-1988_07 |