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Methanol → methyl(5-bromo-1H-inden-2-yl)acetate

HRID 860868
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HRID 860868 반응식
[Br:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH:7]([CH2:12][C:13]([OH:15])=[O:14])[CH:8]2O)=[CH:4][CH:3]=1.S(=O)(=O)(O)O.[CH3:21]O>>[Br:1][C:2]1[CH:10]=[C:9]2[C:5](=[CH:4][CH:3]=1)[CH2:6][C:7]([CH2:12][C:13]([O:15][CH3:21])=[O:14])=[CH:8]2
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참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric Acid2회HCID 67104698(6-bromo-1-hydroxy-2,3-dihydro-1H-inden-2-yl)acetic Acid

생성물 1

HCID 85969236methyl(5-bromo-1H-inden-2-yl)acetate

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온도
10 °C

실험 절차

The product from Example 52B (1.35 g, 5 mmol) in methanol (12 mL) was treated with concentrated sulfuric acid (2 mL) and heated to gentle reflux. After 2 hours, additional sulfuric acid was added (1 mL) and heating was continued for another 2 hours. The mixture was concentrated under vacuum and the residue was diluted with water (15 mL). The mixture was cooled to 10° C., filtered, and the filter cake washed with water (5 mL) and dried to provide the title compound. 1H NMR (CDCl3) δ 3.42 (s, 2H); 3.55 (s, 2H); 3.74 (s, 3H); 6.65 (m, 1H); 7.22-7.31 (m, 2H), 7.44 (m, 1H).

후처리

  1. temperatureheated to gentle reflux
  2. temperatureheating
  3. waitwas continued for another 2 hours
  4. concentrationThe mixture was concentrated under vacuum
  5. additionthe residue was diluted with water (15 mL)
  6. filtrationfiltered
  7. washthe filter cake washed with water (5 mL)
  8. customdried

출처 및 근거

ORD 기록
ord-9a51db15110d4ccfb2bd4098d72c4ab1
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07153889B2

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