Triethylamine → HCID 178515078, 화합물

HRID 323616

반응식

HRID 323616 반응식
CO[C:3]([C:5]1[C:14]([C:15]([O:17]C)=O)=[C:13]([OH:19])[C:12]2[C:7](=[CH:8][C:9]([Cl:20])=[CH:10][CH:11]=2)[N:6]=1)=[O:4].Cl.Cl.[CH2:23]([NH:30][NH2:31])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(N(CC)CC)C>C(O)C>[CH2:23]([N:30]1[C:15](=[O:17])[C:14]2[C:13](=[O:19])[C:12]3[CH:11]=[CH:10][C:9]([Cl:20])=[CH:8][C:7]=3[NH:6][C:5]=2[C:3]([OH:4])=[N:31]1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 146540Benzylhydrazine dihydrochlorideHCID 178418477HCID 178418477, 화합물

생성물 1

HCID 178515078HCID 178515078, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred suspension of dimethyl-7-chloro-4-hydroxyquinoline-2,3-dicarboxylate (5.00 g, 16.90 mM) and benzylhydrazine dihydrochloride (46.15 g, 236.50 mM) in ethanol (100 mL) was added triethylamine (75.8 mL, 541.0 mM). The mixture was heated to give a brown solution which was refluxed for 40 hours during which time a precipitate formed. The suspension was cooled to room temperature and filtered to give the benzylhydrazine salt of the title compound as an impure yellow solid. Multiple crystallizations from ethanolic hydrogen chloride and methanol gave the title compound (0.370 g, 6%) as a white powder, mp 347-350° C.; MS(CI): 354 (M+H).

후처리

  1. temperatureThe mixture was heated
  2. customto give a brown solution which
  3. temperaturewas refluxed for 40 hours during which time a precipitate
  4. customformed
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-f8c16bbecf424a2f81a68afe47b94588
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06214826B1

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