Water → 4-(Dimethylamino)piperidine dihydrochloride
反応式
[ClH:1].Cl.[CH3:3][N:4]([CH3:18])[CH:5]1[CH2:10][CH2:9][N:8](CC2C=CC=CC=2)[CH2:7][CH2:6]1.O>CC(O)C.[C].[Pd]>[ClH:1].[ClH:1].[CH3:3][N:4]([CH3:18])[CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1参加物
5
実験手順
After adding 10% palladium-carbon (2.0 g) to a solution of the crude 4-dimethylamino-1-benzylpiperidine dihydrochloride (30.0 g) in 2-propanol (300 ml)-water (300 ml), the mixture was stirred for 22 hours at room temperature under a hydrogen atmosphere. The catalyst was filtered and washed with 2-propanol. The filtrate was then concentrated. The obtained crystals were suspended in ethanol (50 ml). They were then diluted with diethyl ether (50 ml). The crystals were subsequently filtered and washed with methanol (10 ml). They were then subjected to aeration drying to provide the title compound (16.4 g) as colorless crystals.
後処理
- filtrationThe catalyst was filtered
- washwashed with 2-propanol
- concentrationThe filtrate was then concentrated
- additionThey were then diluted with diethyl ether (50 ml)
- filtrationThe crystals were subsequently filtered
- washwashed with methanol (10 ml)
- customdrying
出典と根拠
- ORDレコード
- ord-21c5d9ace9af48b4810dd4b2b2cac66e
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07531532B2
反応ノート
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