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Acetic Anhydride → Methyl 6-(acetyloxy)-3-bromo-2-methylbenzoate

HRID 1247456
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HRID 1247456 반응식
[Br:1][C:2]1[C:3]([CH3:13])=[C:4]([C:9]([OH:12])=[CH:10][CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].[C:14](OC(=O)C)(=[O:16])[CH3:15]>N1C=CC=CC=1>[C:14]([O:12][C:9]1[C:4]([C:5]([O:7][CH3:8])=[O:6])=[C:3]([CH3:13])[C:2]([Br:1])=[CH:11][CH:10]=1)(=[O:16])[CH3:15]
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참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 21907510Methyl 3-bromo-6-hydroxy-2-methylbenzoate

생성물 1

HCID 21907498Methyl 6-(acetyloxy)-3-bromo-2-methylbenzoate수율 97%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of Example 106B (1.05 g, 4.3 mmol) in pyridine (3 mL) was treated with acetic anhydride (0.82 mL, 8.6 mmol), stirred at room temperature for 2 hours, and partitioned between ethyl acetate and 2N HCl. The organic phase was washed sequentially with aqueous NaHCO3, water, and brine, dried (MgSO4), filtered, and concentrated to give 1.19 g (97% yield) of the desired product. MS (ESI(+)) m/e 304, 306 (M+H)+.

후처리

  1. custompartitioned between ethyl acetate and 2N HCl
  2. washThe organic phase was washed sequentially with aqueous NaHCO3, water, and brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8d2bea2dd5c64e7892d9728472c51cdb
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07129260B2

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