関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1,1,1-Trifluoro-2-propanol | HCID 9774 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1,1,1-Trifluoropropan-2-yl carbonochloridate | HCID 58270348 | — |
反応手順
To a mixture of 1,1,1-trifluoro-2-propanol (114.1 mg, 1.0 mmol, Matrix Scientific) and triphosgene (98 mg, 0.33 mmol, Aldrich) in ethyl ether (10 mL) at −40° C. was added pyridine (80 μL, 1.0 mmol, EMD) in ethyl ether (1.0 mL) dropwise. The reaction mixture was warmed to 0° C. and stirred for 6 h. The flask containing the above reaction mixture was put into a refrigerator overnight and then filtered. The filtrate was concentrated in vacuo in ice both to give a colorless oil which was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08076322B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-4cd0f1305fdd4b8ca6365b36aff1c416 |
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| 出典メモ | uspto-grants-2011_12 |
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