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

HRID 2390397
ノート
印刷プレビュー

反応式

HRID 2390397 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric Acid2 回HCID 67104698(6-bromo-1-hydroxy-2,3-dihydro-1H-inden-2-yl)acetic Acid

生成物 1

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

反応条件

温度
10 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4c1c5aad53c84001bca5d60463554d62
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273767B2

反応ノート

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