Sodium Carbonate → 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one

HRID 1420037노트

반응식

HRID 1420037 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][C:16]([O:18]CC)=O)([O-])=O.O.O.[Cl-].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.Cl>[CH:6]1[C:5]2[N:10]3[CH:14]=[CH:13][CH:12]=[C:11]3[CH2:15][C:16](=[O:18])[NH:1][C:4]=2[CH:9]=[CH:8][CH:7]=1

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 21226388Chloride dihydrateHCID 861831311-(2-Nitrophenyl)-2-pyrroleacetic acid, ethyl ester

생성물 1

HCID 123593406,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one수율 100.9%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

To a solution of 0.8 mmol of 1-(2-nitrophenyl)-2-pyrroleacetic acid, ethyl ester in 3 ml of ethanol is added stannus chloride dihydrate (SnCl2.2H2O) in 2 ml of concentrated hydrochloric acid (with cooling in water bath). The mixture is stirred at room temperature for 5 hours and chilled in an ice bath. To the mixture is added slowly saturated sodium carbonate solution. The solid which precipitates is filtered and the solid washed with water and then extracted with ethyl acetate. The ethyl acetate extract is dried (Na2SO4) and the solvent removed to give 0.16 g of solid which is triturated with ether to give 0.11 g of product as an off-white solid.

후처리

  1. temperaturechilled in an ice bath
  2. customThe solid which precipitates
  3. filtrationis filtered
  4. washthe solid washed with water
  5. extractionextracted with ethyl acetate
  6. extractionThe ethyl acetate extract
  7. dry with materialis dried (Na2SO4)
  8. customthe solvent removed

출처 및 근거

ORD 기록
ord-1e64b0430ebc48788c9613dcb9d12136
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889001

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