Sodium Chloride → Ethyl 7-(cyclohexan-1-on-2-yl)heptanoate

HRID 66983노트

반응식

HRID 66983 반응식
[C:1]1(=[O:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=[O:14].O.[C:18]1(C)C=CC(S(O)(=O)=O)=C[CH:19]=1.C(=O)(O)[O-].[Na+].[Cl-].[Na+]>O.C1C=CC=CC=1.C(O)C>[C:1]1(=[O:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:18][CH3:19])=[O:14]

참가 물질

8

반응물 4

HCID 5234Sodium ChlorideHCID 516892Sodium BicarbonateHCID 521998p-Toluenesulfonic acid monohydrateHCID 204657322-Oxocyclohexaneheptanoic acid

생성물 1

HCID 12848421Ethyl 7-(cyclohexan-1-on-2-yl)heptanoate

시약·촉매·용매 3

HCID 241Benzene용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution of 232 g. of 7-(cyclohexan-1-on-2-yl)heptanoic acid in 2500 ml. of ethanol is refluxed for 4.5 hours with 3.8 g. of p-toluenesulfonic acid monohydrate. The solution is diluted with 200 ml. of benzene, and boiling is continued for 2 hours as 200 ml. of distillate is removed. The volume of the solution is concentrated to 500 ml. After dilution with 500 ml. of ether the solution is extracted with a solution prepared from 50 ml. of saturated sodium bicarbonate, 50 ml. of saturated sodium chloride, and 100 ml. of water. The extract is washed with saturated sodium chloride, dried, and evaporated. The product is purified by distillation to give a liquid, IR 1740 cm-1 (ester carbonyl) and 1715 cm-1 (ketone carbonyl).

후처리

  1. additionThe solution is diluted with 200 ml
  2. customof distillate is removed
  3. concentrationThe volume of the solution is concentrated to 500 ml
  4. extractionof ether the solution is extracted with a solution
  5. customprepared from 50 ml
  6. washThe extract is washed with saturated sodium chloride
  7. customdried
  8. customevaporated
  9. distillationThe product is purified by distillation
  10. customto give a liquid, IR 1740 cm-1 (ester carbonyl) and 1715 cm-1 (ketone carbonyl)

출처 및 근거

ORD 기록
ord-13f40771e7d0407998580d5d4ca0991f
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343949

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