Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-[2-(2-Ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purine-8-carbonyl]piperidine-1-carboxylic acid tert-butyl ester → 4-{1-[2-(2-Ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purin-8-yl]-1-hydroxyethyl}piperidine-1-carboxylic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-[2-(2-Ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purine-8-carbonyl]piperidine-1-carboxylic acid tert-butyl ester | HCID 59605401 | — |
| 반응물 | HCID 178418573 | HCID 178418573 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-{1-[2-(2-Ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purin-8-yl]-1-hydroxyethyl}piperidine-1-carboxylic acid tert-butyl ester | HCID 59605574 | 57% |
반응 단계
To a solution of 4-[2-(2-ethylbenzoimidazol-1-yl)-9-methyl-6-morpholin-4-yl-9H-purine-8-carbonyl]piperidine-1-carboxylic acid tert-butyl ester (177 mg, 0.31 mmol) in THF (3 mL) at 0° C. was added methylmagnesium bromide (130 μL, 0.37 mmol, 3M solution in Et2O) and the resulting mixture stirred for 1 h before further methylmagnesium bromide (130 μL, 0.37 mmol) was added. The resulting mixture was warmed to r.t. and stirred for 16 h then concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, MeOH:EtOAc, 0-10%) affording the title compound as a clear oil (104 mg, 57%). LCMS (method A): RT 3.09 min [M+H]+ 591.2
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08173650B2 |
| 출처 데이터셋 | uspto-grants-2012_05 |
| ORD ID | ord-84a78f0d4cce4863ac93043e0ca7de6a |
| 출처 메모 | uspto-grants-2012_05 |