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Methanol → Methyl 4-bromo-2-methylbutanoate

HRID 1695221
ノート
印刷プレビュー

反応式

HRID 1695221 の反応式
[Br:1][CH2:2][CH2:3][CH:4]([CH3:8])[C:5]([OH:7])=[O:6].[CH3:9]O>OS(O)(=O)=O>[CH3:9][O:6][C:5](=[O:7])[CH:4]([CH3:8])[CH2:3][CH2:2][Br:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 887Methanol2 回HCID 2133316964805-71-6

生成物 1

HCID 11745547Methyl 4-bromo-2-methylbutanoate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

4-Bromo-2-methyl-butyric acid (2.16 g, 1 eq, prepared according to the procedure described in J. Am. Chem. Soc. 1990, 112, 2755) was dissolved in MeOH (10 mL) and a few drops of conc. H2SO4 were added. The reaction was stirred at reflux for 16 hours. After reaction completion, as monitored by LC-MS, MeOH was removed under reduced pressure, the oily residue was diluted with water, the pH adjusted to 9 with 10% NaOH, and the product was extracted with Et2O (2×20 mL) and dried over Na2SO4. The title compound was obtained as a colourless oil (1.29 g, 55% yield) after solvent removal.

後処理

  1. temperatureat reflux for 16 hours
  2. customAfter reaction completion
  3. customwas removed under reduced pressure
  4. additionthe oily residue was diluted with water
  5. extractionthe product was extracted with Et2O (2×20 mL)
  6. dry with materialdried over Na2SO4

出典と根拠

ORDレコード
ord-d5c6090c33fe4d359128fb48e8792ec7
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163729B2

反応ノート

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