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Sodium Hydroxide → methyl N-(3,5-diamino-6-bromopyrazine-2-carbonyl)carbamimidothioate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Methyl-2-thiopseudourea sulfate | HCID 75270 | — |
| 反応物 | Mtbe thf | HCID 22492792 | — |
| 反応物 | 1-(2-Methyl-2-butyl-carbamoyl)prop-1-en-2-yl 3,5-diamino-6-bromopyrazine-2-carboxylate | HCID 86682475 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | methyl N-(3,5-diamino-6-bromopyrazine-2-carbonyl)carbamimidothioate | HCID 140606262 | — |
反応手順
To NaOH (1 mol/l in water; 30 mL; 30 mmol) is added S-methylisothiourea sulfate (5.42 g; 19.5 mmol. The mixture is stirred until complete solution is achieved. TBME/THF (1:1; 100 mL) and then 1-(2-methyl-2-butyl-carbamoyl)prop-1-en-2-yl 3,5-diamino-6-bromopyrazine-2-carboxylate (Intermediate B.62; 7.52 g; 19.5 mmol) are added and the mixture is stirred at r.t. over night, then water (100 mL) is added. The precipitate formed is filtered off with suction, washed with THF/water (1:2) and then dried at 50° C. to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759349B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-f0162b53601240d58aebe7c019b08b19 |
| 出典メモ | uspto-grants-2014_06 |