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

HRID 1455167
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HRID 1455167 반응식
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
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참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344
Dichloromethane
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aea69696d98a498a9eac4c2c44d1489d
출처 데이터셋
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07482362B2

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