Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl 3,3'-(((3-formylphenyl)methylene)bis(sulfanediyl))dipropanoate → Dimethyl 5-(3-(2-(5-chlorobenzoxazol-2-yl) ethenyl)phenyl)-4,6-dithianonanedioate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl 3,3'-(((3-formylphenyl)methylene)bis(sulfanediyl))dipropanoate | HCID 10021188 | — |
| 반응물 | (5 Chlorobenzoxazol-2-yl methyl)triphenylphosphonium bromide | HCID 23055263 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Dimethyl 5-(3-(2-(5-chlorobenzoxazol-2-yl) ethenyl)phenyl)-4,6-dithianonanedioate | HCID 53900955 | — |
반응 단계
To a solution of phosphonium bromide (780 mg) (Step 4) in tetrahydrofuran (THF) (8 mL) at -78° was added dropwise 1 eq. of n-BuLi in hexane. The solution was stirred at -78° for 15 min. Then (545 mg) of the aldehyde (Step 1) in THF (4 mL) was added dropwise and the reaction mixture was stirred at -78° for 1 hour. The reaction mixture was poured into pH 7 buffer, extracted with ethyl acetate, dried and evaporated. The residue was chromatographed on a column of SiO2 using 10:1 toluene/ethyl acetate to afford the title compound, m.p. 66°-67° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04957932 |
| 출처 데이터셋 | uspto-grants-1990_09 |
| ORD ID | ord-79529cb249c848a6b8e08b4fdf46a378 |
| 출처 메모 | uspto-grants-1990_09 |