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Triethylamine → HCID 178423916, 화합물

HRID 1368658
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HRID 1368658 반응식
C(O[C:4](=[O:14])[CH:5]([C:12]#[N:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)C.Cl.Cl.[CH2:17]([NH:24][NH2:25])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[CH2:26](N(CC)CC)C>C(O)C.C(OCC)(=O)C>[NH2:13][C:12]1[N:24]([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:25]=[C:4]([OH:14])[C:5]=1[C:6]1[CH:7]=[CH:8][C:9]([CH3:26])=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 95298Ethyl phenylcyanoacetateHCID 146540Benzylhydrazine dihydrochloride

생성물 1

HCID 178423916HCID 178423916, 화합물수율 20%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirring suspension of ethyl-2-cyano-2-phenylacetate (10.34 g) and benzylhydrazine dihydrochloride (14.87 g) in ethanol (200 ml) at room temperature was added triethylamine (21.27 ml). The reaction mixture was heated to reflux for 24 hours. The solvent was removed under reduced pressure to yield the crude material as a brown oil. This was re-dissolved in ethyl acetate (100 ml) and washed with water (2×75 ml), then dried (MgSO4) and the solvent removed in vacuo to yield a pale brown oil. This was recrystallised from methanol to yield the title product as pale yellow crystals (2.5 g, ca. 20%)

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 hours
  3. customThe solvent was removed under reduced pressure
  4. customto yield the crude material as a brown oil
  5. washwashed with water (2×75 ml)
  6. dry with materialdried (MgSO4)
  7. customthe solvent removed in vacuo
  8. customto yield a pale brown oil
  9. customThis was recrystallised from methanol

출처 및 근거

ORD 기록
ord-e9cea2c5de7443668f7e48ae77ac952e
출처 데이터셋
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06573270B1

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