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Hydrochloric Acid → 4-(4-Chloro-3-fluorobenzyl)morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 4-Chloro-3-Fluorobenzaldehyde | HCID 2724985 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 4-(4-Chloro-3-fluorobenzyl)morpholine | HCID 59543860 | 60.4% |
反応手順
4-Chloro-3-fluorobenzaldehyde (1.0 g, 6.31 mmol), morpholine (0.546 ml, 6.31 mmol) and sodium triacetoxyborohydride (1.938 g, 9.14 mmol) were mixed in dichloroethane (19 ml) and the reaction stirred at ambient temperature under an atmosphere of argon over night. 1M HCl (aq, 25 ml) was added. The mixture was extracted with dichloromethane (×4). The pH was adjusted to ca 12 by adding KOH (s). The mixture was extracted with dichloromethane (×4). The combined organic phases were dried over MgSO4 filtered and concentrated in vacuo to give 4-(4-chloro-3-fluorobenzyl)morpholine (0.875 g, 60%) as a liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08178529B2 |
| 出典データセット | uspto-grants-2012_05 |
| ORD ID | ord-5bff997b060e46a2b820e73238a8ebc3 |
| 出典メモ | uspto-grants-2012_05 |