Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → [(3R)-3-[(2,5-Dichlorophenyl)thio]-3-(2-thiazolyl)propyl]carbamic acid 1,1-dimethylethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 반응물 | 2,5-Dichlorobenzenethiol | HCID 79965 | — |
| 반응물 | [(3S)-3-Hydroxy-3-(2-thiazolyl)propyl]carbamic acid 1,1-dimethylethyl ester | HCID 69799613 | — |
| 용매 | 2-Methylpentane | HCID 7892 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | [(3R)-3-[(2,5-Dichlorophenyl)thio]-3-(2-thiazolyl)propyl]carbamic acid 1,1-dimethylethyl ester | HCID 86759856 | 21% |
반응 단계
To a solution of 2,5-dichlorothiophenol (179 mg, 1 mmol), [(3S)-3-hydroxy-3-(2-thiazolyl)propyl]carbamic acid 1,1-dimethylethyl ester (258 mg, 1 mmol) and triphenylphosphine (315 mg, 1.2 mmol) in dry tetrahydrofuran (30 ml) at 0° C. under nitrogen, was added diisopropyl azodicarboxylate (243 mg, 0.24 ml, 1.2 mmol) dropwise over 5 minutes. The mixture was stirred at room temperature for 16 h, then concentrated in vacuo to leave a crude yellow gum. Flash chromatography (silica, 15% ethyl acetate in isohexane) afforded a clear oil (85 mg, 21%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06953797B2 |
| 출처 데이터셋 | uspto-grants-2005_10 |
| ORD ID | ord-b7d71d8b2993495cb1602eda97538b96 |
| 출처 메모 | uspto-grants-2005_10 |