関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethanesulfonylchloride, 2-chloro- | HCID 15385 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-[4-(Cyclohexyloxy)phenyl]pyrazin-2-amine | HCID 66748148 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-[4-(Cyclohexyloxy)phenyl]-3,4-dihydropyrazino[2,1-c][1,2,4]thiadiazine 2,2-dioxide | HCID 66748512 | 83.2% |
反応手順
A mixture of 3-[4-(cyclohexyloxy)phenyl]pyrazin-2-amine (470 mg) in THF (dry) (25.00 mL) was added to a mixture of NaH (60%, 349 mg) and 2-chloroethanesulfonyl chloride (853 mg) in THF (dry) (25 mL) at room temperature. The mixture was stirred at room temperature overnight and 80° C. for 3 hr. Water was added and THF was removed in vacuo. A precipitate was collected by filtration and washed with water-Et2O to give the title compound (522 mg) as a yellow solid. The solid was crystallized from CH3CN—IPE to give a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08916551B2 |
|---|
| 出典データセット | uspto-grants-2014_12 |
|---|
| ORD ID | ord-a750a6f077ee47ff97c8eccc1a6f5c91 |
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| 出典メモ | uspto-grants-2014_12 |
|---|
