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Potassium Carbonate → HCID 86646688、化合物

HRID 1677438
ノート
印刷プレビュー

反応式

HRID 1677438 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 86646688HCID 86646688、化合物収率 20%

試薬・触媒・溶媒 1

HCID 24386Thionyl Chloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7def7262a2e44fc1a7c871525ebd1110
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08008298B2

反応ノート

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