関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethyl 2-amino-4-chlorothieno(2,3-d)pyrimidine-6-carboxylate | HCID 16096301 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 59519321 | HCID 59519321 | — |
反応手順
To a nitrogen filled flask containing sodium hydride (0.5 mmol, 60% in mineral oil) in anhydrous THF (5 ml) was added benzyl alcohol (0.5 mmol). The suspension was stirred vigorously for 10 minutes until no more gas was evolved before being transferred to a microwave reaction tube containing 2-amino-4-chloro-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (0.129 g, 0.5 mmol). The sealed tube was heated to 90° C. for 5 mins using 300 W in a CEM microwave apparatus (CARE!). The reaction mixture was partitioned between DCM and water, the water layer neutralised and evaporated to dryness in vacuo to leave the pure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08642594B2 |
|---|
| 出典データセット | uspto-grants-2014_02 |
|---|
| ORD ID | ord-180ad0c943c64aadac6321cef049ae07 |
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| 出典メモ | uspto-grants-2014_02 |
|---|