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Methanol → 3-Amino-6-(4-(tert-butoxycarbonyl)piperazin-1-yl)pyrazine-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Tert-butyl 4-(3-methyl-4-oxo-3,4-dihydropteridin-6-yl)piperazine-1-carboxylate | HCID 66745135 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 3-Amino-6-(4-(tert-butoxycarbonyl)piperazin-1-yl)pyrazine-2-carboxylic acid | HCID 66744853 | 34% |
反応手順
Tert-butyl 4-(3-methyl-4-oxo-pteridin-6-yl)piperazine-1-carboxylate (25 g, 72.17 mmol) was stirred in NaOH (250 mL of 10% w/w,) and MeOH (250 mL) overnight at RT. The resulting suspension was concentrated and then acidified with formic acid followed by extraction of the aqueous with DCM. The mixture was treated with water, taken to pH 10 and filtered. The aqueous layer was reacidified and the resulting precipitated product was extracted into DCM and concentrated to give the product as a yellow solid (8 g, 24.74 mmol, 34% Yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08410112B2 |
| 出典データセット | uspto-grants-2013_04 |
| ORD ID | ord-f4b3f02a7da4447a86571d57bc2c52dc |
| 出典メモ | uspto-grants-2013_04 |