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

HRID 1619984노트

반응식

HRID 1619984 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-12d5756b73e949b6bbaf9dbaaec275ee
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772323B2

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