Lithium Hydroxide → 2-Ethyl-2-[1-methyl-2-oxo-2-(2-phenyl-benzoxazol-6-yl)-ethyl]-malonic acid

HRID 1619984ノート

反応式

HRID 1619984 の反応式
[CH2:1]([C:3]([CH:12]([CH3:30])[C:13](=[O:29])[C:14]1[CH:28]=[CH:27][C:17]2[N:18]=[C:19]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[O:20][C:16]=2[CH:15]=1)([C:8]([O:10]C)=[O:9])[C:4]([O:6]C)=[O:5])[CH3:2].[OH-].[Li+]>O1CCOCC1.O>[CH2:1]([C:3]([CH:12]([CH3:30])[C:13](=[O:29])[C:14]1[CH:28]=[CH:27][C:17]2[N:18]=[C:19]([C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)[O:20][C:16]=2[CH:15]=1)([C:4]([OH:6])=[O:5])[C:8]([OH:10])=[O:9])[CH3:2]

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 67464947Dimethyl 2-ethyl-2-[1-methyl-2-oxo-2-(2-phenyl-benzoxazol-6-yl)-ethyl]-malonate

生成物 1

HCID 674631882-Ethyl-2-[1-methyl-2-oxo-2-(2-phenyl-benzoxazol-6-yl)-ethyl]-malonic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

660 mg (1.13 mmol) dimethyl 2-ethyl-2-[1-methyl-2-oxo-2-(2-phenyl-benzoxazol-6-yl)-ethyl]-malonate are dissolved in 20 ml dioxane. Then 170 mg (7.10 mmol) lithium hydroxide, dissolved in 5 ml of water, are added and the mixture is stirred overnight at RT. The reaction mixture is extracted with DCM, the aqueous phase is acidified and extracted again with DCM. Then the org. phase is dried and the solv. is completely eliminated by rotary evaporation i.V. The residue is separated by RP-HPLC (basic).

後処理

  1. additionare added
  2. extractionThe reaction mixture is extracted with DCM
  3. extractionextracted again with DCM
  4. customphase is dried
  5. customThe residue is separated by RP-HPLC (basic)

出典と根拠

ORDレコード
ord-12d5756b73e949b6bbaf9dbaaec275ee
出典データセット
uspto-grants-2014_07
特許番号
US08772323B2

反応ノート

読み込み中…