Sodium Azide → HCID 15690201、化合物

HRID 720760ノート

反応式

HRID 720760 の反応式
[C:1]([N@@:4]1[CH2:6][CH:5]1[CH:7]([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10])(=[O:3])[CH3:2].[N-:14]=[N+:15]=[N-:16].[Na+]>CN(C=O)C.[Cl-].[Cl-].[Zn+2]>[CH2:9]([O:8][CH:7]([O:11][CH2:12][CH3:13])[C@H:5]([NH:4][C:1](=[O:3])[CH3:2])[CH2:6][N:14]=[N+:15]=[N-:16])[CH3:10]

参加物

5

反応物 2

HCID 33557Sodium AzideHCID 21894829HCID 21894829、化合物

生成物 1

HCID 15690201HCID 15690201、化合物収率 62.9%

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
75 °C

実験手順

A mixture containing 3.26 g of 124 and 15 g of sodium azide in 140 ml of DMF was added 140 ml of ZnCl2 (1.0M solution in Et2O), The mixture was stirred at 75° C. for 3 days and then extracted with EtOAc. The organic layer was washed with water, dried over MgSO4 and concentrated. The residue was purified by silica gel chromatography (hexane/EtOAc=3:2) to yield 2.52 g of 125 (62%).

後処理

  1. extractionextracted with EtOAc
  2. washThe organic layer was washed with water
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel chromatography (hexane/EtOAc=3:2)

出典と根拠

ORDレコード
ord-4636defea385480a83b04dbbe418069d
出典データセット
uspto-grants-2006_11
特許番号
US07135578B2

反応ノート

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