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Methanesulfonic Acid → Methanesulfonic acid 3-(4-chlorobenzyl)-1-methyl-2-oxo-cyclopentylmethyl ester

HRID 922737
ノート
印刷プレビュー

反応式

HRID 922737 の反応式
COC([C:5]1([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=2)[CH2:9][CH2:8][C:7]([CH2:11][O:12][S:13]([CH3:16])(=[O:15])=[O:14])([CH3:10])[C:6]1=[O:17])=O.CS(O)(=O)=O>O>[Cl:25][C:22]1[CH:21]=[CH:20][C:19]([CH2:18][CH:5]2[CH2:9][CH2:8][C:7]([CH2:11][O:12][S:13]([CH3:16])(=[O:15])=[O:14])([CH3:10])[C:6]2=[O:17])=[CH:24][CH:23]=1
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 2

HCID 6395Methanesulfonic AcidHCID 867182541-(4-Chlorobenzyl)-3-methanesulfonyloxymethyl-3-methyl-2-oxo-cyclopentancarboxylic acid methyl ester

生成物 1

HCID 86718257Methanesulfonic acid 3-(4-chlorobenzyl)-1-methyl-2-oxo-cyclopentylmethyl ester

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
110 °C

実験手順

To 1.26 g of Compound 3-1-1 obtained in Production Example 2, 0.255 ml of methanesulfonic acid and 88.3 mg of water were added, and the resulting mixture was stirred at 110° C. for 3.5 hours. After the reaction, water was added to the reaction solution thus obtained, and extraction with ethyl acetate was then carried out. The extract was washed with an aqueous solution of sodium hydrogen carbonate and saturated brine. After the organic layer was dried over anhydrous sodium sulfate, the solvent was distilled away.

後処理

  1. additionwere added
  2. additionwas added to the reaction solution
  3. customthus obtained
  4. extractionextraction with ethyl acetate
  5. washThe extract was washed with an aqueous solution of sodium hydrogen carbonate and saturated brine
  6. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled away

出典と根拠

ORDレコード
ord-4834d1e3a0d24272b1d1ff11bbc6667e
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278966B2

反応ノート

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