Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 1-(5-tert-Butyl-isoxazol-3-yl)-3-(4-chloro-benzenesulfonyl)-3-methyl-pyrrolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 반응물 | N-(5-tert-butyl-isoxazol-3-yl)-2-(4-chlorobenzenesulfonyl)-4-hydroxy-2-methyl-butyramide | HCID 58280577 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-(5-tert-Butyl-isoxazol-3-yl)-3-(4-chloro-benzenesulfonyl)-3-methyl-pyrrolidin-2-one | HCID 44609757 | 84% |
반응 단계
To a solution of diethyl azodicarboxylate (0.025 g; 0.14 mmol) in methylene chloride (1 mL) was added triphenylphosphine (0.038 g; 0.14 mmol). The mixture was stirred 20 minutes and N-(5-tert-butyl-isoxazol-3-yl)-2-(4-chlorobenzenesulfonyl)-4-hydroxy-2-methyl-butyramide (0.030 g; 0.072 mmol) in 1 mL methylene chloride was added. After 18 hours the volatiles were removed in vacuo. The residue was purified by silica gel chromatography using ethyl acetate and hexanes as the eluent. Removal of the volatiles from the product-rich fractions provided 0.024 g of product. 1H NMR (CDCl3) δ 7.83 (d, 2H), 7.55 (d, 2H), 6.73 (s, 1H), 4.03 (m, 1H), 3.95 (m, 1H), 3.25 (m, 1H), 2.29 (m, 1H), 1.52 (s, 3H), 1.35 (s, 9H). MS (ESI): m/e 397, 399 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08178568B2 |
| 출처 데이터셋 | uspto-grants-2012_05 |
| ORD ID | ord-55ff04f36fca42b3853c662356f44264 |
| 출처 메모 | uspto-grants-2012_05 |