Sulfuric Acid → HCID 11799027, 화합물

HRID 266124

반응식

HRID 266124 반응식
S(=O)(=O)(O)O.[NH2:6][C:7]1[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH3:28])=[CH:21][C:8]=1[C:9]([C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[C:13]([O:19][CH3:20])[CH:12]=1)=O.[CH3:29][CH2:30][O:31][C:32]([CH2:34][C:35]([CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39])=O)=[O:33]>C(O)(=O)C>[CH3:20][O:19][C:13]1[CH:12]=[C:11]([C:9]2[C:8]3[C:7](=[CH:24][C:23]([O:25][CH3:26])=[C:22]([O:27][CH3:28])[CH:21]=3)[N:6]=[C:35]([CH2:34][C:32]([O:31][CH2:30][CH3:29])=[O:33])[C:37]=2[C:38]([O:40][CH2:41][CH3:42])=[O:39])[CH:16]=[CH:15][C:14]=1[O:17][CH3:18]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 66045Diethyl acetonedicarboxylateHCID 99269672-Amino-4,5,3',4'-tetramethoxybenzophenone

생성물 1

HCID 11799027HCID 11799027, 화합물수율 64.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

Conc. sulfuric acid (1.5 ml) was added to a mixture of 2-amino-4,5,3',4'-tetramethoxybenzophenone (50.0 g), diethyl acetonedicarboxylate (35.0 g) and acetic acid (400 ml), and the mixture was stirred at 100° C. for 2.5 hours. The reaction mixture was concentrated under reduced pressure. The residue was poured into water, neutralized with an aqueous saturated solution of sodium bicarbonate, and extracted with chloroform. The chloroform layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residual crystals were recrystallized from acetone to give ethyl 4-(3,4-dimethoxyphenyl)-6,7-dimethoxy-3-ethoxycarbonylquinoline-2-acetate (48.8 g, 64%). Colorless prisms, mp. 146°-147° C.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionThe residue was poured into water
  3. extractionextracted with chloroform
  4. washThe chloroform layer was washed with water
  5. dry with materialdried over magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residual crystals were recrystallized from acetone

출처 및 근거

ORD 기록
ord-ef881ca9d2034a3ba0e5b9106fd38325
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05650410

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