Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 2-Formyl-3-(tert-butyldimethylsilanyloxy)-5-methoxy-6-methylbenzoic acid allyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 반응물 | 2-Formyl-3-hydroxy-5-methoxy-6-methylbenzoic acid allyl ester | HCID 53735263 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Formyl-3-(tert-butyldimethylsilanyloxy)-5-methoxy-6-methylbenzoic acid allyl ester | HCID 53812279 | 93.8% |
반응 단계
To a solution of 15 g of 2-formyl-3-hydroxy -5-methoxy-6-methylbenzoic acid allyl ester in 0.12 l of N,N-dimethylformamide were added 13.8 g of tert-butyl-dimethylchlorosilane and 12.0 g of triethylamine. The mixture was stirred for 3 h at room temperature and then evaporated in vacuo. The residue was taken up in 0.4 l of ethyl acetate and the solution was washed successively with 1N hydrochloric acid, water and brine. The organic layer was dried over sodium sulfate. The solvent was evaporated in vacuo and the solid residue was recrystallized from hexane to give 20.5 g of 2-formyl-3-(tert-butyl-dimethylsilanyloxy)-5-methoxy-6-methylbenzoic acid allyl ester as white crystals of m.p. 94°-95° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05589473 |
| 출처 데이터셋 | uspto-grants-1996_12 |
| ORD ID | ord-3f38b76d913f4cea9dcc0fe7b75e509f |
| 출처 메모 | uspto-grants-1996_12 |