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Benzylamine → Ethyl cis-(4-amino-3-methoxypiperidino)formate

HRID 846746
ノート
印刷プレビュー

反応式

HRID 846746 の反応式
S1C=CC=C1.[CH3:6][O:7][CH:8]1[C:13](=O)[CH2:12][CH2:11][N:10]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9]1.C1(C[NH2:27])C=CC=CC=1.[H][H]>[Pd].CO.C(O)C>[NH2:27][C@H:13]1[CH2:12][CH2:11][N:10]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9][C@H:8]1[O:7][CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 7504BenzylamineHCID 8030ThiopheneHCID 2724451Ethyl 3-methoxy-4-oxopiperidine-1-carboxylateHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 13677746Ethyl cis-(4-amino-3-methoxypiperidino)formate

試薬・触媒・溶媒 3

HCID 23938Palladium触媒2 回
HCID 702Ethanol溶媒
HCID 887Methanol溶媒

実験手順

To 2 parts of a solution of 2 parts of thiophene in 40 parts of ethanol were added 126 parts of ethyl 3-methoxy-4-oxo-1-piperidinecarboxylate, 70 parts of benzenemethanamine and 400 parts of methanol. The whole was hydrogenated at normal pressure and at room temperature with 5 parts of palladium-on-charcoal catalyst 10%. After up-take of one equivalent of hydrogen, the catalyst was filtered off and hydrogenation was continued with another 5 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. The residue contained some oil drops which were separated, yielding 92.9 parts of ethyl cis-4-amino-3-methoxy-1-piperidinecarboxylate (intermediate 54).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customwere separated

出典と根拠

ORDレコード
ord-08b3ba627c6a411cb51998f6ccb4192f
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05137896

反応ノート

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