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Ethyl Acetate → 5-Bromopyridine-2,3-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 2-Amino-5-bromo-3-nitropyridine | HCID 138878 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | 5-Bromopyridine-2,3-diamine | HCID 691156 | — |
反応手順
A procedure similar to that described in Preparation 42 was repeated, except that 12.0 g of 2-amino-5-bromo-3-nitropyridine (prepared as described in Preparation 56), 62.1 g of tin(II) chloride dihydrate, 1.04 g of sodium borohydride and 300 ml of a 9:1 by volume mixture of ethyl acetate and 2-methyl-2-propanol were used, to give the title compound as a crude product. This crude product was crystallized by trituration with a mixture of ethyl acetate and hexane, to give 7.46 g of the title compound, melting at 135°-137° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624935 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-e2de0ed915b2471ebddf711e17debd8c |
| 出典メモ | uspto-grants-1997_04 |