関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzonitrile | HCID 7505 | — |
| 反応物 | 1,10-Phenanthroline hydrate | HCID 21226 | — |
| 反応物 | 2-Amino-4-bromopyridine | HCID 693282 | — |
| 触媒 | copper(I) bromide | HCID 24593 | — |
| 生成物 | 7-Bromo-2-phenyl-[1,2,4]triazolo[1,5-A]pyridine | HCID 67775500 | 60% |
反応手順
A mixture of 2-amino-4-bromopyridine (5.00 g, 28.9 mmol), copper (I) bromide (207 mg, 1.44 mmol), 1,10-phenanthroline monohydrate (289 mg, 1.44 mmol), and benzonitrile (125 mL) was heated in a 250-mL 3-necked flask to 130° C. During 23 h a gentle flow of air was bubbled through the reaction mixture (80% conversion, HPLC method see below). The dark brown suspension was then cooled to 0-5° C. and filtered. The filter cake was washed with TBME (50 mL) and dried to yield crude 7-bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine (4.87 g, 60%) as a green solid with 97.3% purity (HPLC area-%, HPLC method see below).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09115130B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-5cc4716ae04d4b20baafafdd94bcc884 |
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| 出典メモ | uspto-grants-2015_08 |
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