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Isoamyl Nitrite → Dimethyl 2,6-dichloroterephthalate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isoamyl Nitrite | HCID 8053 | — |
| 反応物 | Dimethyl 2-amino-3,5-dichloroterephthalate | HCID 20714731 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Dimethyl 2,6-dichloroterephthalate | HCID 7730227 | 98.7% |
反応手順
To a solution of dimethyl 2-amino-3,5-dichloroterephthalate (200 g, 0.72 mol) in THF (1 L) at room temperature was slowly added isoamylnitrite (240 mL). The mixture was heated under reflux for 3 hours, cooled to room temperature and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel, eluting with petroleum-diethyl:ether (50:1) to give dimethyl 2,6-dichloroterephthalate (187 g, yield: 98%) as a light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08486950B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-ea54b14529e34b05be5d2e838c3a9823 |
| 出典メモ | uspto-grants-2013_07 |