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

HRID 440748

反応式

HRID 440748 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

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.H2O) 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.

後処理

  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

出典と根拠

ORDレコード
ord-00fed420be7442488c7cf803c774a5ec
出典データセット
uspto-grants-1996_05
特許番号
US05521173

関連ノート

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