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Lithium Hydroxide → HCID 70816435, 화합물

HRID 1843017
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HRID 1843017 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:13]([CH3:19])[C:14]([O:16]CC)=[O:15])[CH:5]=[CH:6][C:7]=1[CH2:8][S:9]([CH3:12])(=[O:11])=[O:10].O1CCCC1.[OH-].[Li+]>O.C(OCC)C>[F:1][C:2]1[CH:3]=[C:4]([CH:13]([CH3:19])[C:14]([OH:16])=[O:15])[CH:5]=[CH:6][C:7]=1[CH2:8][S:9]([CH3:12])(=[O:11])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 70815867HCID 70815867, 화합물

생성물 1

HCID 70816435HCID 70816435, 화합물수율 99%

시약·촉매·용매 2

HCID 962Water용매2회HCID 3283Diethyl Ether용매

실험 절차

To a stirred solution of ethyl 2-(3-fluoro-4-(methylsulfonylmethyl)phenyl)propanoate (950 mg, 3.295 mmol) in co-solvent with tetrahydrofuran and water (1:1) were added lithium hydroxide (236 mg, 9.885 mmol). The reaction mixture was refluxed for overnight, then cooled to room temperature, diluted with water (25 mL) and diethyl ether (25 mL). After phase separation the aqueous layer was acidified by HCl to a pH=3 and extracted with DCM (3×50 mL). The organic layer was dried over magnesium sulfate and filtered. The solvent of the filtrate was removed in vacuo to give 2-(3-fluoro-4-(methylsulfonylmethyl)-phenyl)propanoic acid (846 mg, 99%).

후처리

  1. temperatureThe reaction mixture was refluxed for overnight
  2. customAfter phase separation the aqueous layer
  3. extractionextracted with DCM (3×50 mL)
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. customThe solvent of the filtrate was removed in vacuo

출처 및 근거

ORD 기록
ord-d22bbdd25017468e922f39c2fd5aac51
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946204B2

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