Hydrochloric Acid → 3-Cyclohexylacrylic acid

HRID 1512182노트

반응식

HRID 1512182 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 8082PiperidineHCID 16275Cyclohexanecarboxaldehyde

생성물 1

HCID 2873483-Cyclohexylacrylic acid

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9dc19561e4f542729281dddec5de494f
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217060B2

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