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Potassium Iodide → 4-[10-(4-Carbethoxyphenoxy)decyl]-3,5-heptanedione

HRID 2163418
ノート
印刷プレビュー

反応式

HRID 2163418 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]([C:13](=[O:16])[CH2:14][CH3:15])[C:9](=[O:12])[CH2:10][CH3:11].[OH:17][C:18]1[CH:28]=[CH:27][C:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CC(C)=O>[C:22]([C:21]1[CH:20]=[CH:19][C:18]([O:17][CH2:2][CH2:3][CH2:4][CH2:5][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]([C:13](=[O:16])[CH2:14][CH3:15])[C:9](=[O:12])[CH2:10][CH3:11])=[CH:28][CH:27]=1)([O:24][CH2:25][CH3:26])=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 8434EthylparabenHCID 11430Potassium CarbonateHCID 123634064-(6-Bromohexyl)heptane-3,5-dione

生成物 1

HCID 227536734-[10-(4-Carbethoxyphenoxy)decyl]-3,5-heptanedione

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 26.3 g. (0.0758 mole) of 4-(6-bromohexyl)-3,5-heptanedione, 13.1 g. (0.0787 mole) of ethyl p-hydroxybenzoate, 31.5 g. (0.228 mole) of powdered potassium carbonate, 4 g. of potassium iodide and 500 ml. of acetone was heated at reflux for 36 hours. The reaction mixture was concentrated in vacuo and partitioned between water and methylene dichloride. The organic layer was washed successively with sodium hydroxide solution, water, hydrochloric acid, water and sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solution was concentrated and the residue crystallized and recrystallized from n-pentane to give 4-[10-(4-carbethoxyphenoxy)decyl]-3,5-heptanedione, m.p. 45°-46° C.

後処理

  1. additionA mixture of 26.3 g
  2. temperatureat reflux for 36 hours
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. custompartitioned between water and methylene dichloride
  5. washThe organic layer was washed successively with sodium hydroxide solution, water, hydrochloric acid, water and sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationThe solution was concentrated
  8. customthe residue crystallized
  9. customrecrystallized from n-pentane

出典と根拠

ORDレコード
ord-552d12a6d45e432cb6749a14c8e198ac
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04133959

反応ノート

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