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Methanol → HCID 23094117, 화합물

HRID 2249407
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HRID 2249407 반응식
[C:1]([C:4]1[C:5](=[O:19])[NH:6][N:7]=[C:8]([C:10]2[CH:11]=[CH:12][C:13]3[O:17][CH2:16][CH2:15][C:14]=3[CH:18]=2)[CH:9]=1)([OH:3])=[O:2].S(Cl)(Cl)=O.[CH3:24]O>>[O:17]1[C:13]2[CH:12]=[CH:11][C:10]([C:8]3[CH:9]=[C:4]([C:1]([O:3][CH3:24])=[O:2])[C:5](=[O:19])[NH:6][N:7]=3)=[CH:18][C:14]=2[CH2:15][CH2:16]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 230941044-Carboxy-6-(2,3-dihydro-1-benzofuran-5-yl)-2H-pyridazin-3-one

생성물 1

HCID 23094117HCID 23094117, 화합물

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온도
80 °C

실험 절차

4-Carboxy-6-(2,3-dihydro-1-benzofuran-5-yl)-2H-pyridazin-3-one (5.9 g, 22.8 mmol) was suspended in methanol (100 mL), and thionyl chloride (3 g, 25.1 mmol) was added dropwise to the suspension under cooling with ice, followed by stirring for three hours at 80° C. The temperature of the reaction mixture was reduced to room temperature, and the solvent was removed under reduced pressure. Water was added to the residue under cooling on ice, and the formed precipitates were collected through filtration and washed with water, followed by drying, to thereby yield 4.90 g of the title compound as pale yellow micro-needles (78.8%).

후처리

  1. temperatureunder cooling with ice
  2. customwas reduced to room temperature
  3. customthe solvent was removed under reduced pressure
  4. additionWater was added to the residue
  5. temperatureunder cooling on ice
  6. customthe formed precipitates
  7. filtrationwere collected through filtration
  8. washwashed with water
  9. customby drying

출처 및 근거

ORD 기록
ord-7ab44c3252c04b3fb592bc15ab239603
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314877B2

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