関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-(4,6-Dichloropyrimidin-2-yl)morpholine | HCID 2772068 | — |
| 反応物 | Thiomorpholine 1,1-dioxide | HCID 6484228 | — |
| 反応物 | Tetrahydrofuran ethanol | HCID 21873804 | — |
| 生成物 | 4-(6-Chloropyrimidin-4-yl)morpholine | HCID 796070 | 97% |
反応手順
To a solution of 4-(4,6-dichloropyrimidin-2-yl)morpholine (1.0 equiv.) in EtOH:THF (1:1, 0.25 M) was added thiomorpholine 1,1-dioxide (1.0 equiv.) in one portion. The resulting mixture was heated to 100° C. for 42 h. The resulting mixture was then cooled to RT and concentrated in vacuo to yield an off white solid in The reaction mixture was then concentrated in vacuo and dried under high vacuum over 20 h to yield 4-(6-chloropyrimidin-4-yl)morpholine as a white solid in 97% yield. LCMS (m/z) (M+H)=333.0/334.9, Rt=0.68 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09242969B2 |
|---|
| 出典データセット | uspto-grants-2016_01 |
|---|
| ORD ID | ord-8165ba03c8f2474a8cbd2fc4e09fe009 |
|---|
| 出典メモ | uspto-grants-2016_01 |
|---|