関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | N-Ethyl-N'-(6-nitro-1,3-benzothiazol-2-yl)urea | HCID 9813955 | — |
| 反応物 | 1-Ethyl-5-methyl-3-(6-nitro-1,3-benzothiazol-2-yl)-1,3,5-triazinan-2-one | HCID 21985532 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water ethanol | HCID 19096565 | — |
| 生成物 | N-(6-Cyano-1,3-benzothiazol-2-yl)-N'-(3-pyridylmethyl)urea | HCID 21985518 | — |
反応手順
General procedure for synthesizing 1-ethyl-5-methyl-3-(6-nitro-1,3-benzothiazol-2-yl)-1,3,5-triazinan-2-one: N-Ethyl-N′-(6-nitro-1,3-benzothiazol-2-yl)urea is suspended in an alkanol/water mixture, preferably 1:1 EtOH/H2O at room temperature. A 37% aqueous solution of formaldehyde is added followed by addition of a 2M solution of MeNH2 in MeOH, then about 2 mole equivalents of N-methylmorpholine. The solution is warmed to about 70–85° C., preferably 80° C., then allowed to stir for about 4–24 hours, preferably 4 hours. The slurry is then cooled to room temperature, filtered and washed well with water, dried and the title product is isolated. General Procedure for Grignard Addition:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07091227B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-e8b7ee04ec75448d86e69b5a0568d5fc |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|