関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethyl orthoacetate | HCID 15050 | — |
| 反応物 | Ytterbium triflate | HCID 2733225 | — |
| 反応物 | 2-Amino-5-bromo-4-chlorophenol | HCID 58487100 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Bromo-5-chloro-2-methylbenzoxazole | HCID 58487438 | 80.2% |
反応手順
A mixture of 2-amino-5-bromo-4-chlorophenol (29) (865 mg, 3.89 mmol), trifluoromethanesulfonic acid Ytterbium (III) salt (24 mg, 1% mol) and trimethyl orthoacetate (610 μl, 1.2 eq.) in 3 ml EtOH was heated at 90° C. for 1 h. After cooling down to r.t., off-white needles fell off, which were filtered, washed with MeOH, water and dried to give 791 mg title compound as off-white crystalline solid. Yield: 80.2%; purity>95%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08546403B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
|---|
| ORD ID | ord-b68bf2441fdb47d9bfc9e9bf673751ae |
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| 出典メモ | uspto-grants-2013_10 |
|---|
