Sodium Iodide → HCID 15675385, 화합물

HRID 1461269노트

반응식

HRID 1461269 반응식
Cl[CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5]1=[O:13].[I-].[Na+].[N-:16]=[N+:17]=[N-:18].[Na+]>CN(C)C=O>[N:16]([CH2:2][CH2:3][N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[NH:6][C:5]1=[O:13])=[N+:17]=[N-:18]

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 33557Sodium AzideHCID 36534711-(2-chloroethyl)-1H-benzo[d]imidazol-2(3H)-one2회

생성물 1

HCID 15675385HCID 15675385, 화합물수율 98.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

In 30 ml of dimethylformamide were dissolved 1.5 g of the above 1:1 (approx.) mixture of Compound h and Compound h', 1.5 g (9.9 mmol) of sodium iodide and 5.0 g (76.3 mmol) of sodium azide and the solution was heated at 120° C. for 48 hours. After cooling, the solvent was distilled off and 50 ml of ethyl acetate was added to the residue. The insolubles were filtered off and the filtrate was washed twice with 5% aqueous sodium thiosulfate solution and, then, three times with saturated aqueous sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure to give 1.38 g (98.9%) of 1-(2-azidoethyl)-2,3-dihydro-2-oxo-1H-benzimidazole (Compound i) as light yellow crystals.

후처리

  1. temperatureAfter cooling
  2. distillationthe solvent was distilled off
  3. addition50 ml of ethyl acetate was added to the residue
  4. filtrationThe insolubles were filtered off
  5. washthe filtrate was washed twice with 5% aqueous sodium thiosulfate solution
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-4f74d634d08c41cd81e874e4c2c34ed1
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075301

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