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Ethyl chloroformate → Biphenyl-2,2'-diyl diethyl dicarbonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | (1,1'-Biphenyl)-2,2'-diol | HCID 15731 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | Biphenyl-2,2'-diyl diethyl dicarbonate | HCID 58288702 | — |
反応手順
To a round-bottom flask is charged biphenyl-2,2′-diol (7.45 g, 40 mmol) and pyridine (50 mL). The flask is immersed in an ice-water bath and ethyl chloroformate (9.48 mL, 100 mmol) is added dropwise. After gradually warming to room temperature, the mixture is stirred overnight. The volatiles are removed in vacuo, and the residue is suspended in 100 mL of ethyl acetate. After filtration, the filtrate is concentrated and purified by flash chromatography. The product is obtained as a colorless oil. Yield: 5.0 g; 1H NMR (500 MHz, CDCl3, ppm) δ 7.23-7.44 (m, 8H), 4.13 (q, 4H), 1.19 (t, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08633126B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-2b56f5493d7444798e5c727b7761c58b |
| 出典メモ | uspto-grants-2014_01 |