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Sodium Chloride → Methyl 3-bromo-5-fluoro-4-hydroxybenzoate

HRID 521534
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HRID 521534 반응식
[Br:1]Br.[CH3:3][O:4][C:5](=[O:14])[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([F:13])[CH:7]=1.C(OC)(=O)C.S([O-])([O-])=O.[Na+].[Na+].[Cl-].[Na+]>C(Cl)Cl.C(O)(=O)C.O>[CH3:3][O:4][C:5](=[O:14])[C:6]1[CH:7]=[C:8]([F:13])[C:9]([OH:12])=[C:10]([Br:1])[CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 5234Sodium ChlorideHCID 6584Methyl AcetateHCID 24408BromineHCID 24437Sodium SulfiteHCID 7019368Methyl 3-fluoro-4-hydroxybenzoate

생성물 1

HCID 57467610Methyl 3-bromo-5-fluoro-4-hydroxybenzoate

시약·촉매·용매 3

HCID 176
Acetic Acid
용매
HCID 962Water용매2회
HCID 6344Dichloromethane용매

실험 절차

During 30 min, 5.64 g (35.27 mmol) of bromine were added to a solution of 5.00 g (29.39 mmol) of 3-fluoro-4-hydroxy-benzoic acid methyl ester in 30 ml of DCM and 30 ml of acetic acid at 0° C. After stirring overnight, 200 ml of methyl acetate were added. The resulting solution was extracted with a solution of 7.56 g (60 mmol) of sodium sulfite in 50 ml of water, a saturated sodium chloride solution and water. The organic phase was dried over sodium sulfate, filtered and evaporated. The resulting white solid (7.2 g) was used in the next step without further purification.

후처리

  1. dry with materialThe organic phase was dried over sodium sulfate
  2. filtrationfiltered
  3. customevaporated
  4. customThe resulting white solid (7.2 g) was used in the next step without further purification

출처 및 근거

ORD 기록
ord-59bd07b0164a4532950e03b82be06beb
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09328071B2

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