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Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | 2,6-Difluorobenzamide | HCID 87439 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 2,6-Difluorobenzoyl isocyanate | HCID 2733369 | — |
反応手順
Oxalyl chloride (5.5 g) was added slowly to a suspension of 2,6-difluorobenzamide (6.0 g) in 1,2-dichloroethane maintained at a temperature within the range -10° to -5° C. When the addition was complete the mixture was allowed to warm to the ambient temperature, and then gradually heated to the reflux temperature and maintained thereat for a period of 16 hours. The solvent was then removed by evaporation under reduced pressure and the residual oil purified by distillation to yield 2,6-difluorobenzoyl isocyanate, b.p. 60°-61°/0.7 mm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04150158 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-f779bab063b2461595cd6647fbefa252 |
| 出典メモ | uspto-grants-1979_04 |