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Methyl iodide → methyl 3-fluoro-2-formylbenzoate

HRID 365070
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HRID 365070 반응식
[F:1][C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]([OH:12])[O:5][C:6]2=[O:7].[C:13](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[F:1][C:2]1[C:3]([CH:4]=[O:12])=[C:8]([CH:9]=[CH:10][CH:11]=1)[C:6]([O:5][CH3:13])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 13555831HCID 13555831, 화합물

생성물 1

HCID 13752496methyl 3-fluoro-2-formylbenzoate수율 95.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A stirred mixture containing 7.36 g 4-fluoro-3-hydroxyphthalide, 18.15 g potassium carbonate and 11 mL methyl iodide in 125 mL acetone is heated at reflux for two hours. After stirring overnight at room temperature, the mixture is filtered and concentrated. The residue is dispersed in 200 mL ether, filtered and the filtrate concentrated to give 7.6 g residue which is used directly without further purification. The nmr spectrum of this material is consistent with that expected for the desired product.

후처리

  1. temperatureis heated
  2. temperatureat reflux for two hours
  3. filtrationthe mixture is filtered
  4. concentrationconcentrated
  5. additionThe residue is dispersed in 200 mL ether
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated

출처 및 근거

ORD 기록
ord-39d89443bea04959ac5d2f4d9021f4e1
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04608079

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