Methanol → Ethyl 4-(aminomethyl)-4-hydroxypiperidine-1-carboxylate

HRID 579781

反応式

HRID 579781 の反応式
[OH:1][C:2]1([CH2:13][N+:14]([O-])=O)[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:3]1.CO.[H][H]>[Pd].C(O)(=O)C>[NH2:14][CH2:13][C:2]1([OH:1])[CH2:3][CH2:4][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:6][CH2:7]1

参加物

6

反応物 3

HCID 887MethanolHCID 22708806Ethyl 4-hydroxy-4-(nitromethyl)-1-piperidinecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 14049029Ethyl 4-(aminomethyl)-4-hydroxypiperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

A mixture of 73 parts of ethyl 4-hydroxy-4-(nitromethyl)-1-piperidinecarboxylate, 400 parts of methanol and 150 parts of acetic acid was hydrogenated in the Parr-apparatus with 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. To the residue was added crushed ice and the whole was alkalized with potassium hydroxide. The aqueous phase was salted out with potassium carbonate and the product was extracted with benzene. The extract was dried, filtered and evaporated, yielding 63.5 parts of ethyl 4-(aminomethyl)-4-hydroxy-1-piperidinecarboxylate; mp. ±82° C. (intermediate 6).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. additionTo the residue was added
  4. customcrushed ice
  5. extractionthe product was extracted with benzene
  6. customThe extract was dried
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-57e94454633f4bb884ce95040a1c1a8f
出典データセット
uspto-grants-1988_06
特許番号
US04749702

関連ノート

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