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Methanol → Methyl 6-fluoro-3-iodo-2-methylbenzoate

HRID 1948669
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HRID 1948669 반응식
C[Si](C=[N+]=[N-])(C)C.[F:8][C:9]1[C:14]([C:15]([OH:17])=[O:16])=[C:13]([CH3:18])[C:12]([I:19])=[CH:11][CH:10]=1.[CH3:20]O>C1C=CC=CC=1>[F:8][C:9]1[C:14]([C:15]([O:17][CH3:20])=[O:16])=[C:13]([CH3:18])[C:12]([I:19])=[CH:11][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 167693TrimethylsilyldiazomethaneHCID 594505486-Fluoro-3-iodo-2-methylbenzoic acid

생성물 1

HCID 59450535Methyl 6-fluoro-3-iodo-2-methylbenzoate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Trimethylsilyldiazomethane solution (2 M in Hexane) (18 mL, 35 mmol) was added dropwise to a stirred solution of the product of Step A (7.3 g, 33.2 mmol) in benzene containing 20% of methanol (total: 100 mL) at room temperature until solution retained a yellow color. The mixture was concentrated to remove the organic solvent. The remaining oil was poured over a silica gel plug in a 60-mL filter frit funnel and eluting with 200 mL of hexane containing 10% ethyl acetate. The filtrate was then concentrated to dryness to give the title compound as a bright yellow oil.

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후처리

  1. concentrationThe mixture was concentrated
  2. customto remove the organic solvent
  3. additionThe remaining oil was poured over a silica gel plug in a 60-mL
  4. filtrationfilter frit funnel
  5. washeluting with 200 mL of hexane containing 10% ethyl acetate
  6. concentrationThe filtrate was then concentrated to dryness

출처 및 근거

ORD 기록
ord-02f00273b72c43bfbe4c0149769ce382
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399507B2

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