関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 2-(5-Methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-yl)acetic acid | HCID 853753 | — |
| 反応物 | N-(Carbamoylmethyl)-beta-alanine ethylester | HCID 22737577 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | dichloromethane N,N-dimethylformamide | HCID 22350042 | — |
| 生成物 | N-(Carbamoylmethyl)-N-(thymin-1-ylacetyl)-beta-alanine ethyl ester | HCID 22737569 | 61.4% |
反応手順
DhbtOH (9.37 g, 57.4 mmol), N1-thyminyl acetic acid (10.57 g, 57.4 mmol) and CH2Cl2 (100 mL) were added to a solution of N-(carbamoylmethyl)-β-alanine ethylester (10.0 g, 57.4 mmol) in dry DMF (100 mL). The solution was cooled to 0° C. in an ice bath and a solution of DCC (1.90 g, 9.18 mmol) in DMF/CH2Cl2 (100 mL, 1:1 v/v) was added dropwise within 20 minutes. The ice bath was removed and after stirring for 1 hour at room temperature. The reaction mixture was filtered and the precipitate (DCU) was rinsed with CH2Cl2 (50 mL). The organic solution and the CH2Cl2 rinse were combined. A colorless precipitate formed overnight which was filtered and rinsed with CH2Cl2. The precipitate was dried in vacuo to give 12.0 g (61%) (mp 207-208° C.) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06713602B1 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-e79c5c77798049f2af95b4ccefdf6e6b |
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| 出典メモ | uspto-grants-2004_03 |
|---|
