Hydrochloric Acid → 3-Cyclohexylacrylic acid

HRID 1512182

反応式

HRID 1512182 の反応式
[C:1](O)(=O)[CH2:2][C:3]([OH:5])=[O:4].[CH:8]1(C=O)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.N1CCCCC1.Cl>N1C=CC=CC=1.O>[CH:8]1([CH:1]=[CH:2][C:3]([OH:5])=[O:4])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 8082PiperidineHCID 16275Cyclohexanecarboxaldehyde

生成物 1

HCID 2873483-Cyclohexylacrylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049Pyridine溶媒

実験手順

A solution of malonic acid (30 g, 0.29 mol), cyclohexanecarbaldehyde (17.3 ml, 0.14 mol) and piperidine (2.9 ml, 0.029 mol) in pyridine (90 ml) was stirred at 70° C. for 18 h. The resulting solution was allowed to cool to room temperature and then water (200 ml) was added. The resulting solution was acidified to pH 2 (litmus) using 1N HCl. The acidic aqueous solution was extracted thrice with ethyl acetate. The ethyl acetate extracts were pooled, washed successively with water, brine, dried over sodium sulfate, filtered and concentrated to yield 3-cyclohexyl-acrylic acid.

後処理

  1. extractionThe acidic aqueous solution was extracted thrice with ethyl acetate
  2. washwashed successively with water, brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-9dc19561e4f542729281dddec5de494f
出典データセット
uspto-grants-2012_07
特許番号
US08217060B2

関連ノート

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