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Morpholine, 4-chloro- → 4,5-Dichloro-2-methoxybenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine, 4-chloro- | HCID 90067 | — |
| 反応物 | 4-Chloro-o-anisic acid | HCID 93682 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 4,5-Dichloro-2-methoxybenzoic acid | HCID 21180343 | 16.9% |
反応手順
To an ice cold solution of 4-chloro-2-methoxybenzoic acid (1.0 g, 5.36 mmol) in trifluoroacetic acid (7 ml) was added N-chloromorpholine (0.67 g, 5.5 mmol) dropwise, maintaining the internal temperature below 10° C. After stirring overnight at room temperature the trifluoroacetic acid was removed in vacuo and the residue partitioned between ethyl acethate and water. The organic layer was dried over magnesium sulfate, concentrated in vacuo and the residue recrystallised from methanol to afford the title compound as a white solid (200 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06110934 |
| 出典データセット | uspto-grants-2000_08 |
| ORD ID | ord-c5ff3b1a7fd742159e25e5bec5dd1b66 |
| 出典メモ | uspto-grants-2000_08 |