Sodium Carbonate → HCID 21463486, 화합물

HRID 1940594노트

반응식

HRID 1940594 반응식
[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

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 21463488HCID 21463488, 화합물

생성물 1

HCID 21463486HCID 21463486, 화합물수율 15%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%)

후처리

  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

출처 및 근거

ORD 기록
ord-2ba7ffd4f1db48af8b719b65808e2445
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700818

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