Potassium Carbonate → Ethyl 2-(2-ethynyl-4-fluoro-5-nitrophenyl)acetic acid

HRID 1930308노트

반응식

HRID 1930308 반응식
[F:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([CH2:11][C:12]([O:14]CC)=[O:13])=[C:4]([C:17]#[C:18][Si](C)(C)C)[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH2:29]1COC[CH2:30]1.CO>CCOCC>[CH2:29]([CH:11]([C:5]1[CH:6]=[C:7]([N+:8]([O-:10])=[O:9])[C:2]([F:1])=[CH:3][C:4]=1[C:17]#[CH:18])[C:12]([OH:14])=[O:13])[CH3:30]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 21899815MeOH tetrahydrofuranHCID 69088386Ethyl 2-(4-fluoro-5-nitro-2-(2-(trimethylsilyl)ethynyl)phenyl)acetate

생성물 1

HCID 86620161Ethyl 2-(2-ethynyl-4-fluoro-5-nitrophenyl)acetic acid

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Ethyl 2-(4-fluoro-5-nitro-2-(2-(trimethylsilyl)ethynyl)phenyl)acetate (0.85 g, 2.6 mmol) and K2CO3 (3.6 g) were dissolved in THF/MeOH (5:1, 30 mL) and the mixture was stirred overnight at RT. The reaction mixture was diluted with Et2O and washed with sat'd NH4Cl solution. The organic layer was dried (MgSO4), filtered, and concentrated. The residue was purified by silica gel column chromatography to obtain ethyl 2-(2-ethynyl-4-fluoro-5-nitrophenyl)acetic acid.

후처리

  1. washwashed with sat'd NH4Cl solution
  2. dry with materialThe organic layer was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-9f691b33b9fd434fa712e9f15105e55d
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188113B2

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