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p-Toluenesulfonic acid → HCID 20367264, 화합물

HRID 460925
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인쇄 미리보기

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HRID 460925 반응식
C([O:3][C:4](=O)[CH:5]=[C:6]([NH2:10])OCC)C.C1(C)C=CC(S(O)(=O)=O)=CC=1.[Cl:23][C:24]1[C:32]([Cl:33])=[CH:31][CH:30]=[CH:29][C:25]=1[CH2:26][NH:27][NH2:28]>C(O)C>[NH2:10][C:6]1[NH:28][N:27]([CH2:26][C:25]2[CH:29]=[CH:30][CH:31]=[C:32]([Cl:33])[C:24]=2[Cl:23])[C:4](=[O:3])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 278451beta-Aminobeta-ethoxyacrylic acid ethyl esterHCID 20367233[(2,3-Dichlorophenyl)methyl]hydrazine

생성물 1

HCID 20367264HCID 20367264, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

16.7 g of β-amino-β-ethoxyacrylic acid ethyl ester and 1 g of p-toluenesulphonic acid were dissolved in 100 ml of ethanol and 20.2 g of 2,3-dichlorobenzylhydrazine were added. After standing overnight at room temperature, the precipitate which had formed was filtered off and dissolved in 2 N sodium hydroxide solution. The alkaline solution was again extracted with ether and subsequently slightly acidified with dilute acetic acid. Hereupon the compound identified above precipitated and after recrystallisation from ethanol the melting point was 161°-162° C. Yield: 11 g (40%).

후처리

  1. customthe precipitate which had formed
  2. filtrationwas filtered off
  3. dissolutiondissolved in 2 N sodium hydroxide solution
  4. extractionThe alkaline solution was again extracted with ether
  5. customabove precipitated
  6. customafter recrystallisation from ethanol the melting point was 161°-162° C

출처 및 근거

ORD 기록
ord-a6873184c9034a6f84046500e698afc1
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04061653

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