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Benzaldehyde → 4-Benzylpiperazine-2-carboxamide

HRID 35317
ノート
印刷プレビュー

反応式

HRID 35317 の反応式
S1C=CC=C1.[CH:6](=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[NH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH:15]1[C:20]([NH2:22])=[O:21].[H][H]>[Pt].CO.C(O)C>[C:7]1([CH2:6][N:17]2[CH2:18][CH2:19][NH:14][CH:15]([C:20]([NH2:22])=[O:21])[CH2:16]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
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 240BenzaldehydeHCID 8030ThiopheneHCID 3019914Piperazine-2-carboxamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 142302664-Benzylpiperazine-2-carboxamide収率 55%

試薬・触媒・溶媒 3

HCID 23939Platinum触媒
HCID 702
Ethanol
溶媒
HCID 887Methanol溶媒

実験手順

To 1 part of a solution of 2 parts of thiophene in 40 parts of ethanol were added 2.2 parts of benzaldehyde, 2.6 parts of 2-piperazinecarboxamide and 120 parts of methanol. The whole was hydrogenated at normal pressure and at room temperature with 2 parts of platinum-on-charcoal catalyst 5%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The solid residue was boiled in 64 parts of acetonitrile. The mixture was filtered and the filtrate was allowed to crystallize at room temperature. The product was filtered off and dried, yielding 2.4 parts (55%) of 4-(phenylmethyl)-2-piperazinecarboxamide; mp. 168.3° C. (intermediate 36).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. filtrationThe mixture was filtered
  4. customto crystallize at room temperature
  5. filtrationThe product was filtered off
  6. customdried

出典と根拠

ORDレコード
ord-9f193ad997424c4c8d6552e9e1529713
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04766125

反応ノート

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