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Diethyl Ether → Methyl 6-bromo-3-hydroxypicolinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Methyl 3-Hydroxy-2-pyridinecarboxylate | HCID 819341 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 6-bromo-3-hydroxypicolinate | HCID 22175135 | 70.7% |
反応手順
To a mechanically stirred solution of methyl 3-hydroxypicolinate (30.6 g) in water (800 mL) was slowly added bromine (32 g) over a 30 minute period. After the addition was complete, stirring was continued for an additional hour. Ether (300 mL) was added and stirring continued until all the solids had dissolved. The organic layer was separated and the aqueous phase extracted with ether (200 mL). The organic phases were combined, dried (MgSO4) and the solvent evaporated to give 32.8 g of methyl 6-bromo-3-hydroxypicolinate as an off-white solid. Recrystallization from methanol/water gave an analytical sample, m.p. 115-117° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706740B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-409760df93f049d191399ae263fb4d8d |
| 出典メモ | uspto-grants-2004_03 |