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Sodium Hydroxide → HCID 58398461、化合物

HRID 1879416
ノート
印刷プレビュー

反応式

HRID 1879416 の反応式
[F:1][CH:2]([CH3:35])[CH2:3][N:4]([S:26]([C:29]1[S:30][CH:31]=[C:32]([CH3:34])[N:33]=1)(=[O:28])=[O:27])[C:5]1[CH:13]=[C:12]2[C:8]([CH2:9][CH2:10][CH2:11]2)=[CH:7][C:6]=1[O:14][CH2:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]([O:22]C)=[O:21])=[CH:18][CH:17]=1.[OH-].[Na+:37]>C1COCC1.CO>[F:1][CH:2]([CH3:35])[CH2:3][N:4]([S:26]([C:29]1[S:30][CH:31]=[C:32]([CH3:34])[N:33]=1)(=[O:28])=[O:27])[C:5]1[CH:13]=[C:12]2[C:8]([CH2:9][CH2:10][CH2:11]2)=[CH:7][C:6]=1[O:14][CH2:15][C:16]1[CH:17]=[CH:18][C:19]([C:20]([O-:22])=[O:21])=[CH:24][CH:25]=1.[Na+:37]
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

5

反応物 2

HCID 14798Sodium HydroxideHCID 58398472methyl 4-{[(6-{(2-fluoropropyl)[(4-methyl-1,3-thiazol-2-yl)sulfonyl]amino}-2,3-dihydro-1H-inden-5-yl)oxy]methyl}benzoate

生成物 1

HCID 58398461HCID 58398461、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

351 mg of methyl 4-{[(6-{(2-fluoropropyl)[(4-methyl-1,3-thiazol-2-yl)sulfonyl]amino}-2,3-dihydro-1H-inden-5-yl)oxy]methyl}benzoate was dissolved in 5.00 mL of THF and 5.00 mL of methanol, and 2.03 mL of a 1 M aqueous sodium hydroxide solution was added thereto, followed by stirring at 50° C. for 4 hours. The reaction liquid was concentrated under reduced pressure, to the obtained residue were added a 5% w/v aqueous citric acid solution and chloroform, and the organic layer was separated using a Phase Separate-filter manufactured by Isotute, and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was dissolved in 5.00 mL of ethanol, and 0.765 mL of an aqueous sodium hydroxide solution was added thereto, followed by concentration under reduced pressure. The obtained crude product was crystallized by the addition of isopropanol/ethanol, collected by filtration, and dried under reduced pressure to obtain 268 mg of sodium 4-{[(6-{(2-fluoropropyl)[(4-methyl-1,3-thiazol-2-yl)sulfonyl]amino}-2,3-dihydro-1H-inden-5-yl)oxy]methyl}benzoate.

後処理

  1. customThe reaction liquid
  2. concentrationwas concentrated under reduced pressure, to the obtained residue
  3. additionwere added a 5% w/v aqueous citric acid solution and chloroform
  4. customthe organic layer was separated
  5. filtrationSeparate-filter
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated
  8. dissolutionthe obtained residue was dissolved in 5.00 mL of ethanol
  9. addition0.765 mL of an aqueous sodium hydroxide solution was added
  10. concentrationfollowed by concentration under reduced pressure
  11. customThe obtained crude product
  12. customwas crystallized by the addition of isopropanol/ethanol
  13. filtrationcollected by filtration
  14. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6562713d499948788947e8858646aba2
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08314240B2

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