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Methanol → HCID 23094117、化合物

HRID 2249407
ノート
印刷プレビュー

反応式

HRID 2249407 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

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

生成物 1

HCID 23094117HCID 23094117、化合物

反応条件

温度
80 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-7ab44c3252c04b3fb592bc15ab239603
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314877B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート