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Water → Methyl 4-bromo-2-chlorobenzeneacetate

HRID 1641534
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HRID 1641534 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=[O:10])=[C:4]([Cl:12])[CH:3]=1.[C:13](=O)([O-])[O-].[K+].[K+].IC.O>CN(C)C=O>[CH3:13][O:10][C:9](=[O:11])[CH2:8][C:5]1[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][C:4]=1[Cl:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 534036172-(4-Bromo-2-chlorophenyl)acetic acid

생성물 1

HCID 57624630Methyl 4-bromo-2-chlorobenzeneacetate수율 102.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매
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실험 절차

To a solution of 4-bromo-2-chlorophenylacetic acid (240 g) of Reference Example 15 in N,N-dimethylformamide (3000 mL) were added potassium carbonate (399 g) and iodomethane (164 g) at 7° C., and the mixture was stirred at the same temperature for 3 hr and stirred at room temperature for 19 hr. The reaction mixture was poured into water, and partitioned and extracted with ethyl acetate. The organic layer was washed 3 times with 25% brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give the title compound (259 g) as a brown oil.

후처리

  1. stirringstirred at room temperature for 19 hr
  2. custompartitioned
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed 3 times with 25% brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b00b01ea797248cab5ae2490c0dd9845
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08114902B2

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