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Sodium hydride → (8S)-9-[(2,6-difluorophenyl)carbonyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 反応物 | (S)-8-(Morpholin-4-yl)-2-(trifluoromethyl)-1,2,3,4-tetrahydropyrimido[1,2-a]pyrimidin-6-one | HCID 136238743 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (8S)-9-[(2,6-difluorophenyl)carbonyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4H-pyrimido[1,2-a]pyrimidin-4-one | HCID 49854503 | 5% |
反応手順
The product is prepared according to the procedure described in Example 18, using 300 mg of (8S)-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one (Example 1e), 47 mg of sodium hydride and 174 mg of 2,6-difluorobenzoyl chloride in 4 ml of tetrahydrofuran. After three successive purifications by silica chromatography (eluent: CH2Cl2/MeOH; gradient of 100/0 to 98/02 then 98/1 and 98/2), 22 mg of (8S)-9-[(2,6-difluorophenyl)carbonyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4 H-pyrimido[1,2-a]pyrimidin-4-one are obtained in the form of a white solid, the characteristics of which are the following:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846670B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-41bbb78abb91412da4d8d3b3333d25e9 |
| 出典メモ | uspto-grants-2014_09 |