Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → HCID 22397507, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 3-Chloro-4-fluorophenol | HCID 75790 | — |
| 반응물 | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 22397507 | HCID 22397507 | 105.2% |
반응 단계
DEAD (0.43 ml) was added to a solution of triphenylphosphine (0.72 g), 3-chloro-4-fluorophenol (0.403 g) and 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (0.5 g) in THF at RT. The resulting mixture was stirred overnight, HCl in dioxan (2 ml of 4M) was added and the mixture stirred at RT overnight. The mixture was then evaporated to dryness and triethylamine (5 ml) was added. The mixture was evaporated and the residue was dissolved in methanol (110 ml), placed onto a SCX cartridge (Varian, 10 g, SCX cartridge available from International Sorbent Technology Isolute® Flash SCX-2) and eluted: first with methanol then with 10% NH3 in methanol. The basic fractions were combined and evaporated to give the product as an oil (0.6 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07179922B2 |
| 출처 데이터셋 | uspto-grants-2007_02 |
| ORD ID | ord-80db32a74d1f4ba1a5830b7a80dae201 |
| 출처 메모 | uspto-grants-2007_02 |