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Octanoic Acid → 5-Octanoyl-2,2-dimethyl-1,3-dioxane-4,6-dione

HRID 1455167
ノート
印刷プレビュー

反応式

HRID 1455167 の反応式
C1(N=C=NC2CCCCC2)CCCCC1.[C:16](O)(=[O:24])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23].[CH3:26][C:27]1([CH3:35])[O:34][C:32](=[O:33])[CH2:31][C:29](=[O:30])[O:28]1>CN(C)C1C=CN=CC=1.ClCCl>[CH3:26][C:27]1([CH3:35])[O:34][C:32](=[O:33])[CH:31]([C:16](=[O:24])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[C:29](=[O:30])[O:28]1
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 3

HCID 379Octanoic AcidHCID 10868DicyclohexylcarbodiimideHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 3567035-Octanoyl-2,2-dimethyl-1,3-dioxane-4,6-dione収率 95%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344
Dichloromethane
溶媒

実験手順

N,N′-Dicyclohexylcarbodiimide (11 mmol) was added to a stirred solution of octanoic acid (10 mmol) and 4-dimethylaminopyridine (12 mmol) in dry dichloromethane (40 ml). The mixture was stirred at room temperature for 1 hour and Meldrum's acid (10 mmol) was added. The stirring was continued at room temperature overnight. The solvent was removed in vacuum and the residue redissolved in ethyl acetate and filtered. The filtrate was washed with 2 M HCl solution and dried over MgSO4. The solvent was rotary evaporated to obtain the title product as an oil in 95% yield and was used without purification in the next step.

後処理

  1. waitThe stirring was continued at room temperature overnight
  2. customThe solvent was removed in vacuum
  3. dissolutionthe residue redissolved in ethyl acetate
  4. filtrationfiltered
  5. washThe filtrate was washed with 2 M HCl solution
  6. dry with materialdried over MgSO4
  7. customThe solvent was rotary evaporated

出典と根拠

ORDレコード
ord-aea69696d98a498a9eac4c2c44d1489d
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482362B2

反応ノート

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