Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Nitrobenzenesulfonyl chloride → 17-Ethyl-1,14-dihydroxy-12-{2'-[4"-hydroxy-3"-(o-nitrobenzenesulfonyl)cyclohexyl]-1'-methylvinyl}-23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9]octacos-18-ene-2,3,10,16-tetraone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Nitrobenzenesulfonyl chloride | HCID 15540 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 17-Ethyl-1,14-dihydroxy-12-[2'(3",4"-dihydroxycyclohexyl)-1'-methylvinyl]-23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9]octacos-18-ene-2,3,10,16-tetraone | HCID 57203845 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 17-Ethyl-1,14-dihydroxy-12-{2'-[4"-hydroxy-3"-(o-nitrobenzenesulfonyl)cyclohexyl]-1'-methylvinyl}-23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9]octacos-18-ene-2,3,10,16-tetraone | HCID 57060669 | — |
반응 단계
To a cooled solution (0° C.) of 17-ethyl-1,14-dihydroxy-12-[2'-(3",4"-dihydroxycyclohexyl)-1'-methylvinyl]-23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9 ]octacos-18-ene-2,3,10,16-tetraone (787mg) in dry methylene chloride (15 ml) is added diisopropylethyl amine (492.4 mg) followed by o-nitrobenzenesulfonyl chloride (281 mg) and a catalytic amount of N,N-dimethylaminopyridine. The yellow solution is stirred at room temperature under a nitrogen atmosphere for 3 hr., and then quenched with sat'd aqueous sodium bicarbonate. Organic layer is washed (water, sat'd NaHCO3, sat'd NaCl), dried (anhydrous Na2SO4) and the solvent is removed in vacuo. Chromatography on silica gel gives the title compounds.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05208228 |
| 출처 데이터셋 | uspto-grants-1993_05 |
| ORD ID | ord-ae8387d53024474eb3bc9d421cec0140 |
| 출처 메모 | uspto-grants-1993_05 |