Lithium hydroxide, monohydrate → 2-(4-Iodophenyl)propanoic acid

HRID 330812

反応式

HRID 330812 の反応式
O.[OH-].[Li+].C[O:5][C:6](=[O:16])[CH:7]([C:9]1[CH:14]=[CH:13][C:12]([I:15])=[CH:11][CH:10]=1)[CH3:8]>O.C1COCC1.CO>[I:15][C:12]1[CH:11]=[CH:10][C:9]([CH:7]([CH3:8])[C:6]([OH:16])=[O:5])=[CH:14][CH:13]=1

参加物

6

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 10589545Methyl 2-(4-iodophenyl)propanoate

生成物 1

HCID 152255732-(4-Iodophenyl)propanoic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

0.610 g (14.6 mmol) lithiumhydroxide monohydrate in 15 mL water are added to 2.12 g (7.31 mmol) 2-(4-iodo-phenyl)-propionic acid methyl ester (Bioorg. Med. Chem. Lett. 2010, 20, 896) in 20 mL THF and 12 mL MeOH at 0° C. Cooling is removed and the mixture is stirred at rt for 2 h. After that time, the mixture is acidified with 1 N HCl to pH˜1 and extracted with DCM. The organic layer is washed with brine, dried over sodium sulphate and the solvent is evaporated. The product is used without further purification in Example IV.1

後処理

  1. temperatureCooling
  2. customis removed
  3. extractionextracted with DCM
  4. washThe organic layer is washed with brine
  5. dry with materialdried over sodium sulphate
  6. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-9688652224b341aeb2d3783198eb34d3
出典データセット
uspto-grants-2014_11
特許番号
US08877754B2

関連ノート

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