Pyridine → 1,1,1-Trifluoropropan-2-yl carbonochloridate
反応式
[F:1][C:2]([F:7])([F:6])[CH:3]([OH:5])[CH3:4].[Cl:8][C:9](Cl)([O:11]C(=O)OC(Cl)(Cl)Cl)Cl.N1C=CC=CC=1>C(OCC)C>[Cl:8][C:9]([O:5][CH:3]([CH3:4])[C:2]([F:7])([F:6])[F:1])=[O:11]参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a mixture of 1,1,1-trifluoro-2-propanol (114.1 mg, 10 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 colorless oil which was used directly in the next step.
後処理
- additionThe flask containing the above reaction mixture
- customwas put into a refrigerator overnight
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo in ice both to colorless oil which
出典と根拠
- ORDレコード
- ord-3863166ae333446ea655f4b72feb6f7e
- 出典データセット
- uspto-grants-2012_07
- 特許番号
- US08232404B2
反応ノート
読み込み中…