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Water → 6-Butyryl-7,8-dimethyl-4-oxo-1,4-dihydroquinoline-2-carboxylic acid

HRID 1632507
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HRID 1632507 반응식
C[O:2][C:3]([C:5]1[NH:6][C:7]2[C:12]([C:13](=[O:15])[CH:14]=1)=[CH:11][C:10]([C:16](=[O:20])[CH2:17][CH2:18][CH3:19])=[C:9]([CH3:21])[C:8]=2[CH3:22])=[O:4].[OH-].[K+].O>CO>[C:16]([C:10]1[CH:11]=[C:12]2[C:7](=[C:8]([CH3:22])[C:9]=1[CH3:21])[NH:6][C:5]([C:3]([OH:4])=[O:2])=[CH:14][C:13]2=[O:15])(=[O:20])[CH2:17][CH2:18][CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 13234025HCID 13234025, 화합물

생성물 1

HCID 132340266-Butyryl-7,8-dimethyl-4-oxo-1,4-dihydroquinoline-2-carboxylic acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6.1 g of 6-butyryl-7,8-dimethyl-4-oxo-1,4-dihydroquinoline-2-carboxylic acid methyl ester are heated under reflux for 4 hours together with 3.66 g of potassium hydroxide, 1.46 ml of water and 64.4 ml of methanol. The reaction mixture is concentrated to dryness by evaporation, partitioned between ethyl acetate and water, the aqueous phases are acidified and the precipitated crystals are filtered with suction and washed with water. The 6-butyryl-7,8-dimethyl-4-oxo-1,4-dihydroquinoline-2-carboxylic acid obtained in this manner melts at 267°-269° after recrystallisation from methanol/ethanol.

후처리

  1. concentrationThe reaction mixture is concentrated to dryness by evaporation
  2. custompartitioned between ethyl acetate and water
  3. filtrationthe precipitated crystals are filtered with suction
  4. washwashed with water

출처 및 근거

ORD 기록
ord-a6098c2fe75e4ae98a95a0db71df69cd
출처 데이터셋
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04476132

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