1-Chloroethyl chloroformate → 4,4-Difluoropiperidine hydrochloride
反応式
[Cl:1]C(OC(Cl)C)=O.C([N:15]1[CH2:20][CH2:19][C:18]([F:22])([F:21])[CH2:17][CH2:16]1)C1C=CC=CC=1>C(Cl)Cl>[ClH:1].[F:21][C:18]1([F:22])[CH2:19][CH2:20][NH:15][CH2:16][CH2:17]1参加物
4
実験手順
In an argon atmosphere, 1-chloroethyl chloroformate (2.62 mL) was added dropwise to the above-obtained N-benzyl-4,4-difluoropiperidine (4.66 g) in methylene chloride (93 mL) at 0° C., and the resultant mixture was stirred at 55° C. for 2 hours, and then cooled in air. The reaction solvent was removed under reduced pressure, and the residue in methanol (93 mL) was refluxed under heat for 4 hours, and then cooled in air. The reaction solvent was removed under reduced pressure, to thereby give the title compound as a solid (3.03 g, 87%).
後処理
- temperaturecooled in air
- customThe reaction solvent was removed under reduced pressure
- temperaturethe residue in methanol (93 mL) was refluxed
- temperatureunder heat for 4 hours
- temperaturecooled in air
- customThe reaction solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-cc5da8b7849f47a09569b63285e0781c
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07622471B2
反応ノート
読み込み中…