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Triphenylphosphine → Dibenzyl azodicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Dibenzyl azodicarboxylate | HCID 5387121 | — |
| 反応物 | 7-Allyl-8-chloro-3-pentyl-1H-purine-2,6(3H,7H)-dione | HCID 59299557 | — |
| 反応物 | 3-{3-[(4-Chlorophenyl)methyl]-1,2,4-oxadiazol-5-yl}-1-propanol | HCID 66812939 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Dibenzyl azodicarboxylate | HCID 5387121 | 177.5% |
| 生成物 | 8-Chloro-1-(3-{3-[(4-chlorophenyl)methyl]-1,2,4-oxadiazol-5-yl}propyl)-3-pentyl-3,7-dihydro-1H-purine-2,6-dione | HCID 59395525 | — |
反応手順
To a solution of 8-chloro-3-pentyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (0.10 g, 0.34 mmol), 3-{3-[(4-chlorophenyl)methyl]-1,2,4-oxadiazol-5-yl}-1-propanol (0.086 g, 0.34 mmol) and triphenylphosphine (0.186 g, 0.69 mmol) in THF (5 ml) was added dibenzylazodicarboxylate (0.204 g, 0.68 mmol) and the solution stirred for 18 h. The solution was then concentrated and the residues chromatographed over silica (20 g, SPE) eluting with DCM initially then DCM/Et2O mixtures to yield the title compound contaminated with dibenzylazodicarboxylate by-products (0.18 g). Material used crude in deprotection step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08143264B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-981292021ff24f748c5004279100e538 |
| 出典メモ | uspto-grants-2012_03 |