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Triethylamine → 3-((methylamino)carbonyl)-N-(2,4,6-trichlorophenyl)-1-piperazineacetamide

HRID 1073153
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HRID 1073153 반응식
[CH3:1][NH:2][C:3]([CH:5]1[CH2:10][NH:9][CH2:8][CH2:7][NH:6]1)=[O:4].Cl[CH2:12][C:13]([NH:15][C:16]1[C:21]([Cl:22])=[CH:20][C:19]([Cl:23])=[CH:18][C:17]=1[Cl:24])=[O:14].C(N(CC)CC)C>COCCO>[CH3:1][NH:2][C:3]([CH:5]1[NH:6][CH2:7][CH2:8][N:9]([CH2:12][C:13]([NH:15][C:16]2[C:17]([Cl:24])=[CH:18][C:19]([Cl:23])=[CH:20][C:21]=2[Cl:22])=[O:14])[CH2:10]1)=[O:4]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 311222-chloro-N-(2,4,6-trichlorophenyl)acetamideHCID 14722545N-Methylpiperazine-2-carboxamide

생성물 1

HCID 147225463-((methylamino)carbonyl)-N-(2,4,6-trichlorophenyl)-1-piperazineacetamide수율 24.4%

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

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온도
60 °C

실험 절차

A mixture of 15.33 parts of N-methyl-2-piperazinecarboxamide, 27.2 parts of 2-chloro-N-(2,4,6-trichlorophenyl)acetamide, 9.8 parts of N,N-diethylethanamine and 300 parts of 2-methoxyethanol was stirred for 3 hours at 60° C. The reaction mixture was evaporated. The residue was taken up in a small amount of water and treated with sodium carbonate. The product was extracted three times with dichloromethane. The combined extracts were dried, filtered and evaporated. The residue was crystallized from acetonitrile. The product was filtered off (the filtrate was set aside) and dried, yielding a first fraction of 9.27 parts (24.4%) of 3-((methylamino)carbonyl)-N-(2,4,6-trichlorophenyl)-1-piperazineacetamide.

후처리

  1. customThe reaction mixture was evaporated
  2. additiontreated with sodium carbonate
  3. extractionThe product was extracted three times with dichloromethane
  4. customThe combined extracts were dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was crystallized from acetonitrile
  8. filtrationThe product was filtered off (the filtrate
  9. customdried

출처 및 근거

ORD 기록
ord-a48e90cd4289448397265026f8de01c7
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04968684

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