Hydrochloric Acid → cis-Pyrrolidine-3,4-diyldimethanol
反応式
C1(C[N:8]2[CH2:12][C@H:11]([CH2:13][OH:14])[C@H:10]([CH2:15][OH:16])[CH2:9]2)C=CC=CC=1.Cl>CO.[OH-].[OH-].[Pd+2]>[NH:8]1[CH2:12][C@H:11]([CH2:13][OH:14])[C@H:10]([CH2:15][OH:16])[CH2:9]1参加物
5
実験手順
To a solution of crude [(cis)-1-(phenylmethyl)-3,4-pyrrolidinediyl]dimethanol (2.5 g) in MeOH (50 mL) was added conc HCl (0.2 mL) followed by Pearlmans catalyst (700 mg). The resulting suspension was hydrogenated for 48 hours at 50 psi on a Parr shaker, after which time a further 700 mg of the catalyst was added. Hydrogenation for another 72 hours at 50 psi resulted in completion of the reaction. Removal of the catalyst by filtration and evaporation of the solvents under reduced pressure yielded (cis)-3,4-pyrrolidinediyldimethanol (970 mg, 7.4 mmol). LCMS: (M+H)+: Not detected.
後処理
- customHydrogenation for another 72 hours at 50 psi resulted in completion of the reaction
- customRemoval of the catalyst
- filtrationby filtration and evaporation of the solvents under reduced pressure
出典と根拠
- ORDレコード
- ord-437a70d861434db5a8fdcc3694cd0c9f
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07893056B2
反応ノート
読み込み中…