Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → HCID 14031259, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 반응물 | Phenoxazine | HCID 67278 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 14031259 | HCID 14031259 | — |
반응 단계
5 Grams of phenoxazine was dissolved in 100 ml of dry tetrahydrofuran, then 1.63 g of 50% sodium hydride in mineral oil was added and the mixture refluxed for 30 minutes. Then 6.19 g of t-butyldimethylsilyl chloride in dimethylformamide (2 ml) and tetrahydrofuran (8 ml) was added and reflux was continued for five more minutes. The reaction was quenched by the addition of water, the organic layer was separated and dried over sodium sulfate. Then the solvent was removed under reduced pressure and the residue purified by column chromatography (silica as solid phase, hexane:ethylacetate (95:5) as mobile phase). N-t-butyldimethylsilylphenoxane had a melting point of 57° C. after crystallization from pentane.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04707473 |
| 출처 데이터셋 | uspto-grants-1987_11 |
| ORD ID | ord-ff27321f287a4e1ead576b4f6dfe71a7 |
| 출처 메모 | uspto-grants-1987_11 |