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

HRID 973007ノート

反応式

HRID 973007 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-45073944bad14b9ca3a66b56a1fcb8e8
出典データセット
uspto-grants-1977_10
特許番号
US04054604

反応ノート

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