Carbonic acid sodium salt (1:2) → 6,7-dihydro-5H-pyrrolo[1,2-a][1,5]benzodiazepin-6-one

HRID 975868笔记

反应方程式

HRID 975868 反应方程式
[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

参与物

6

反应物 3

HCID 10340Carbonic acid sodium salt (1:2)HCID 21226388Chloride dihydrateHCID 861831311-(2-Nitrophenyl)-2-pyrroleacetic acid, ethyl ester

产物 1

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

试剂、催化剂与溶剂 2

HCID 313盐酸溶剂HCID 702乙醇溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-b5172ad0d3ca4ddd911d921613488d4c
来源数据集
uspto-grants-1997_03
专利号
US05610156

反应笔记

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