Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl morpholine oxide → Tert-butyl 4-oxo-6-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)spiro[chroman-2,4'-piperidine]-1'-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl morpholine oxide | HCID 82029 | — |
| 반응물 | Tert-butyl 4-hydroxy-6-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)spiro[chroman-2,4'-piperidine]-1'-carboxylate | HCID 136136847 | — |
| 촉매 | HCID 178419074 | HCID 178419074 | — |
| 용매 | Acetonitrile tetrahydrofuran | HCID 22177404 | — |
| 생성물 | Tert-butyl 4-oxo-6-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)spiro[chroman-2,4'-piperidine]-1'-carboxylate | HCID 136058068 | — |
반응 단계
To a solution of 1.0 g of tert-butyl 4-hydroxy-6-(5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl)spiro[chroman-2,4′-piperidine]-1′-carboxylate in 40 ml of THF-CH3CN (1:1) at r.t. were added 2.0 g of MS 4A, 435 mg of NMO, and 88 mg of TPAP, and the reaction mixture was stirred at r.t. overnight. The mixture was filtered through a Celite pad, washed with CHCl3 and CHCl3-MeOH (9:1), and the filtrate was concentrated in reduced pressure. The residue was purified by column chromatography on silica gel using a mixture of hexane-AcOEt (100/0-0/100) as eluent to give the intended compound as a colorless solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08093389B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-0fe58e149f9b4e03a7baf5149d62f739 |
| 출처 메모 | uspto-grants-2012_01 |