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Pyridine → Phenyl 1H-benzo[d][1,2,3]triazol-5-ylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | HCID 178507366 | HCID 178507366 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Phenyl 1H-benzo[d][1,2,3]triazol-5-ylcarbamate | HCID 178521835 | 57% |
反応手順
To a solution of 1H-benzo[d][1,2,3]triazol-5-amine (1.85 g, 13.8 mmol, Alfa Aesar) in THF (10 mL) and CH3CN (8 mL) was added pyridine (1.34 mL, 16.6 mmol) followed by phenyl chloroformate (2.27 mL, 14.5 mmol) slowly. The reaction was stirred overnight. The reaction was concentrated to give an oil, which was partitioned between CH2Cl2 and water. The organic layer was dried using a SPE phase separator and concentrated to give a solid. This was taken up in CH2Cl2 and the precipitate was filtered to give the desired product (2.0 g, 57%) which was used without purification. MS M+1: 256.06.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08044052B2 |
| 出典データセット | uspto-grants-2011_10 |
| ORD ID | ord-89dbd0b464a34d7d86d04e9bdc9844bb |
| 出典メモ | uspto-grants-2011_10 |