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Triethylamine → 2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylthieno[3,2-d]pyrimidin-4(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,3,4,5-Tetrahydrobenzo[f][1,4]thiazepine 1-oxide | HCID 19608203 | — |
| 反応物 | 2-chloro-6-methylthieno[3,2-d]pyrimidin-4(3H)-one | HCID 136359787 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylthieno[3,2-d]pyrimidin-4(3H)-one | HCID 136359788 | 81.1% |
反応手順
2-Chloro-6-methylthieno[3,2-d]pyrimidin-4(3H)-one (3.01 g, 15 mmol) was dissolved in toluene (50 mL), followed by addition of 6,7,8,9-tetrahydro-5-thia-8-aza-benzocycloheptene-5-oxide (3.39 g, 18.7 mmol), triethylamine (6 mL, 43 mmol). Then the solution was heated to reflux overnight. The suspension was filtrated and the solid was washed by methanol to afford 4.2 g of 2-(1-oxido-2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylthieno[3,2-d]pyrimidin-4(3H)-one (yield was 81.1%) as a slight brown solid. MS obsd. (ESI+) [(M+H)+] 346.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08604019B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-546760932c7d4ce7851aa7b19caadd55 |
| 出典メモ | uspto-grants-2013_12 |