Sodium Azide → HCID 15690201, 화합물

HRID 1835840노트

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HRID 1835840 반응식
[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]

참가 물질

5

반응물 2

HCID 33557Sodium AzideHCID 21894829HCID 21894829, 화합물

생성물 1

HCID 15690201HCID 15690201, 화합물수율 62.9%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 6228Dimethylformamide용매

반응 조건

온도
75 °C

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-5267013bec4247398448a6636463cd18
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06774140B1

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