Methanol → HCID 68839439、化合物

HRID 660600ノート

反応式

HRID 660600 の反応式
C([O:5][C:6](=[O:31])/[CH:7]=[CH:8]/[C:9]1[CH:14]=[CH:13][C:12]([N:15]2[CH2:19][C:18](=[O:20])[NH:17][S:16]2(=[O:22])=[O:21])=[C:11]([O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:10]=1)(C)(C)C.CO.[OH-].[Na+]>C1COCC1>[CH2:24]([O:23][C:11]1[CH:10]=[C:9](/[CH:8]=[CH:7]/[C:6]([OH:31])=[O:5])[CH:14]=[CH:13][C:12]=1[N:15]1[CH2:19][C:18](=[O:20])[NH:17][S:16]1(=[O:22])=[O:21])[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 68842437HCID 68842437、化合物

生成物 1

HCID 68839439HCID 68839439、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (E)-3-[3-benzyloxy-4-(1,1,4-trioxo-1,2,5-thiadiazolidin-2-yl)-phenyl]-acrylic acid tert-butyl ester (2.2 g, 5.18 mmol) in THF (14 mL)/MeOH (7 mL) is added 3.5 mL (20.7 mmol) of 6N NaOH solution and the mixture is stirred at RT for 18 h. The solvent is removed under reduced pressure and water is added to the residue. The mixture is acidified with 1N HCl and is extracted with methylene chloride. The organic phase is washed with water and brine then is dried over sodium sulfate. The solvent is removed under reduced pressure to give the title compound as a reddish solid: ): (M−1)−=387.

後処理

  1. customThe solvent is removed under reduced pressure and water
  2. additionis added to the residue
  3. extractionis extracted with methylene chloride
  4. washThe organic phase is washed with water and brine
  5. dry with materialthen is dried over sodium sulfate
  6. customThe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-1dd63cb94ba4404e9391fdbbee1855ad
出典データセット
uspto-grants-2011_12
特許番号
US08084448B2

反応ノート

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