Sodium Carbonate → HCID 21463486、化合物

HRID 1940594ノート

反応式

HRID 1940594 の反応式
[NH2:1][C:2]1[C:10]2[O:9][CH2:8][CH2:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.Cl.[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18]Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18][NH:1][C:2]1[C:10]2[O:9][CH2:8][CH2:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 21463488HCID 21463488、化合物

生成物 1

HCID 21463486HCID 21463486、化合物収率 15%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 7-amino-5-nitro-2,3-dihydrobenzofuran (D4) (2 g) in ethanol (60 ml) was treated with 2-dimethylaminoethyl chloride hydrochloride (3.36 g) and excess sodium carbonate (6 g), and heated at reflux for 4 days under argon. The solvent was evaporated under reduced pressure, and the residue partitioned between water and chloroform. The organic phase was dried (Na2SO4) and evaporated under reduced pressure to leave an oil which was chromatographed on silica, eluting with methanol and chloroform to give the title compound as a viscous red oil (416 mg, 15%)

後処理

  1. temperatureheated
  2. temperatureat reflux for 4 days under argon
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue partitioned between water and chloroform
  5. dry with materialThe organic phase was dried (Na2SO4)
  6. customevaporated under reduced pressure
  7. customto leave an oil which
  8. customwas chromatographed on silica
  9. washeluting with methanol and chloroform

出典と根拠

ORDレコード
ord-2ba7ffd4f1db48af8b719b65808e2445
出典データセット
uspto-grants-1997_12
特許番号
US05700818

反応ノート

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