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Water → Methyl 3-t-butyl-5-iodo-4-methoxybenzoate

HRID 385031
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HRID 385031 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([I:16])[C:14]=1[OH:15])[C:8]([O:10][CH3:11])=[O:9])([CH3:4])([CH3:3])[CH3:2].[C:17](=O)([O-])[O-].[K+].[K+].COS(=O)(=O)OC.O>CN(C)C=O>[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([I:16])[C:14]=1[O:15][CH3:17])[C:8]([O:10][CH3:11])=[O:9])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 12084815Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate

생성물 1

HCID 68108746Methyl 3-t-butyl-5-iodo-4-methoxybenzoate수율 96%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate (2.77 g) was dissolved in N,N-dimethylformamide (50 mL), and potassium carbonate (12.0 g) and dimethylsulfuric acid (4.1 mL) were added to the solution, and then the mixture was stirred at room temperature for 16 hours. Water was added to the reaction solution, and then the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (2.77 g) as a brown crystal.

후처리

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-a3fdc6c5d6c8440d9f6023c43467b14b
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367843B2

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