Ethanol → 2-Ethenylquinoxaline

HRID 456599

反応式

HRID 456599 の反応式
S(OC)(OC)(=O)=O.[N:8]1S[N:11]=[C:10]2[CH:13]=[C:14](CC#N)[CH:15]=[CH:16][C:9]=12.C(N([CH2:25][CH3:26])CC)C.[CH2:27](O)[CH3:28]>O>[CH:27]([C:25]1[CH:26]=[N:8][C:9]2[C:10](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=1)=[CH2:28]

参加物

6

反応物 4

HCID 702EthanolHCID 6497Dimethyl SulfateHCID 8471TriethylamineHCID 695224455-Cyanomethylbenz-2,1,3-thiadiazole

生成物 1

HCID 218034212-Ethenylquinoxaline収率 66%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Dimethyl sulfate (1.07 ml, 11.3 mmol) was added dropwise, while maintaining the mixture temperature below 40° C., to a solution of amine (a) (2.6 g 11.3 mmol) in ethanol (3 ml). The thick mixture was diluted with water (15 ml) then triethylamine (1.13 ml) was added and the mixture heated for 2 hours on a water bath. After cooling the mixture was extracted with diethyl ether. The organic phase was dried over magnesium sulfate, concentrated to dryness and the residue was chromatographed on silica eluting with heptane-ethyl acetate (3-1) to give the product (1.16 g, 66%).

後処理

  1. temperaturewhile maintaining the mixture temperature below 40° C.
  2. temperaturethe mixture heated for 2 hours on a water bath
  3. temperatureAfter cooling the mixture
  4. extractionwas extracted with diethyl ether
  5. dry with materialThe organic phase was dried over magnesium sulfate
  6. concentrationconcentrated to dryness
  7. customthe residue was chromatographed on silica eluting with heptane-ethyl acetate (3-1)

出典と根拠

ORDレコード
ord-3a2816ff52c14b7685cc57f5e516a080
出典データセット
uspto-grants-2007_03
特許番号
US07186730B2

関連ノート

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