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Potassium Carbonate → HCID 86646688, 화합물

HRID 1677438
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HRID 1677438 반응식
[CH3:1][O:2][CH2:3][C:4]([CH3:9])([CH3:8])[C:5]([OH:7])=O.[CH3:10][O:11][NH:12][CH3:13].Cl.C([O-])([O-])=O.[K+].[K+]>S(Cl)(Cl)=O>[CH3:1][O:2][CH2:3][C:4]([CH3:9])([CH3:8])[C:5]([N:12]([O:11][CH3:10])[CH3:13])=[O:7]
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 30175063-Methoxy-2,2-dimethylpropanoic acid

생성물 1

HCID 86646688HCID 86646688, 화합물수율 20%

시약·촉매·용매 1

HCID 24386Thionyl Chloride용매

실험 절차

A solution of 3-methoxy-2,2-dimethyl-propionic acid (1.0 g, 7.6 mmol) in thionyl chloride (5 ml) was heated to 50° C. for 16 hours. The reaction mixture was concentrated to a yellow residue and then dissolved in DCM (15 ml). O,N-Dimethyl-hydroxylamine-hydrogen chloride (886 mg, 9.1 mmol) and powdered K2CO3 (2.2 g, 16 mmol) were added, and the reaction mixture was stirred at room temperature for 16 hours. The reaction mixture was filtered through a filter funnel, and the filtrate was collected and concentrated giving a white semisolid. The crude product was purified by silica gel chromatography using 20-50% EtOAc in hexanes as eluant providing 260 mg (20%) of 3,N-dimethoxy-2,2,N-trimethyl-propionamide as a colorless oil.

후처리

  1. concentrationThe reaction mixture was concentrated to a yellow residue
  2. dissolutiondissolved in DCM (15 ml)
  3. filtrationThe reaction mixture was filtered through a filter funnel
  4. customthe filtrate was collected
  5. concentrationconcentrated
  6. customgiving a white semisolid
  7. customThe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-7def7262a2e44fc1a7c871525ebd1110
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008298B2

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