化工社化工社 化学情報印刷レポート · 研究参考用
Methyl Isocyanate → HCID 54387530、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)-phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde oxime | HCID 136352416 | — |
| 触媒 | Di-n-butyl diacetoxy tin | HCID 9798523 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 54387530 | HCID 54387530 | 71.2% |
反応手順
A mixture of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde oxime (1.5 g), methyl isocyanate (0.705 g), and dibutyltin diacetate (2 drops) was stirred in dichloromethane at 20° C. in a sealed bottle for 2 days. The mixture was partitioned between water and dichloromethane, the organic layer dried (Na2SO4) and evaporated and the residue crystallized from ethyl acetate/hexane to give 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazole-3-carboxaldehyde O-(N-methylcarbamoyl)oxime (1.22 g) m.p.146-147° C. Compound 18.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06638956B2 |
| 出典データセット | uspto-grants-2003_10 |
| ORD ID | ord-6c8d6e7aadb845f79974c931c71e91a8 |
| 出典メモ | uspto-grants-2003_10 |