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Benzaldehyde → 4-Benzylpiperazine-2-carboxamide

HRID 35317
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반응식

HRID 35317 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 240BenzaldehydeHCID 8030ThiopheneHCID 3019914Piperazine-2-carboxamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 142302664-Benzylpiperazine-2-carboxamide수율 55%

시약·촉매·용매 3

HCID 23939Platinum촉매
HCID 702
Ethanol
용매
HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9f193ad997424c4c8d6552e9e1529713
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04766125

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