Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isopropanol → 2,6-dichloro-9-(propan-2-yl)-9H-purine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isopropanol | HCID 3776 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2,6-Dichloropurine | HCID 5324412 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,6-dichloro-9-(propan-2-yl)-9H-purine | HCID 11218490 | 49% |
반응 단계
Add DEAD (4.7 g, 27.09 mmol) slowly to a solution of 2,6-dichloropurine (1, 5 g, 26.5 mmol), triphenylphosphine (1 1.75 g, 44.5 mmol) and isopropyl alcohol (2b, 10 ml) in THF (100 ml), and stir at room temperature for 24 hours. Concentrate the reaction mixture, dissolve the residue in DCM (20 ml) and filter to remove the unwanted solids. Load the filtrate onto a 90 gram silica gel column (Biotage), and elute with DCM/acetone (95:5). Concentrate the desired fractions to give 3.0 grams of 2,6-dichloro-9-isopropyl-9H-purine (3b). 1H-NMR (CDCl3): δ 8.2(s, 1H), 4.95 (pentet, 1H), 1.63 (d, 6H)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07429595B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-111d6fea9fff42cfb2b4ea6057a5ce78 |
| 출처 메모 | uspto-grants-2008_09 |