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1-Phenethylamine → (+)-Ethyl cis-3-methoxy-4-[(1-phenylethyl)amino]-1-piperidinecarboxylate

HRID 345576
ノート
印刷プレビュー

反応式

HRID 345576 の反応式
Cl.ClCC1C=CC(N2C=CN=C2)=CC=1.[CH3:15][O:16][CH:17]1[C:22](=O)[CH2:21][CH2:20][N:19]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:18]1.[CH3:29][CH:30]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[NH2:31].S1C=CC=C1.[H][H]>C(O)C.[Pd].CO>[CH3:15][O:16][C@H:17]1[C@@H:22]([NH:31][CH:30]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH3:29])[CH2:21][CH2:20][N:19]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:18]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 74081-PhenethylamineHCID 8030ThiopheneHCID 2724451Ethyl 3-methoxy-4-oxopiperidine-1-carboxylateHCID 197946621-[4-(chloromethyl)phenyl]-1H-imidazole hydrochlorideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 67914576(+)-Ethyl cis-3-methoxy-4-[(1-phenylethyl)amino]-1-piperidinecarboxylate
収率 51%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 887Methanol溶媒

実験手順

A solution of 20 parts of ethyl 3-methoxy-4-oxo-1-piperidinecarboxylate, 12 parts of (-)-α-methylbenzenemethanamine, 2 parts of a solution of thiophene in ethanol 4% and 200 parts of methanol was hydrogenated at normal pressure and at room temperature with 4 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated in vacuo. The residue was purified by HPLC using a mixture of hexane, trichloromethane and methanol (50:49.5:0.5 by volume) as eluent. The pure A-fractions were collected and the eluent was evaporated, yielding 15.62 parts (51%) of (-)-ethyl cis-3-methoxy-4-[(1-phenylethyl)amino]-1-piperidinecarboxylate as a residue (intermediate 103).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was purified by HPLC
  4. additiona mixture of hexane, trichloromethane and methanol (50:49.5:0.5 by volume) as eluent
  5. customThe pure A-fractions were collected
  6. customthe eluent was evaporated

出典と根拠

ORDレコード
ord-57194a63cb7d4511a02e1f1861792cf9
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05057525

反応ノート

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