Dimethylformamide → NSC265263

HRID 1657870노트

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HRID 1657870 반응식
[N-:1]=[N+:2]=[N-:3].[Na+].CS(O[CH2:10][CH2:11][N:12]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][N:14]=[C:13]1[CH3:20])(=O)=O.CN(C)C=O.C(=O)([O-])[O-].[K+].[K+]>O>[N:1]([CH2:10][CH2:11][N:12]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][N:14]=[C:13]1[CH3:20])=[N+:2]=[N-:3]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 33557Sodium AzideHCID 931412-(2-Methyl-5-nitro-1-imidazolyl)ethyl methanesulfonate

생성물 1

HCID 3246588NSC265263

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 10 parts of sodium azide is added a solution of 32 parts of 2-(5-nitro-2-methyl-1-imidazolyl)ethyl methanesulfonate (Ger. Pat. No. 2,030,314) in 250 parts of warm N,N-dimethylformamide. The resultant mixture is stirred at approximately 50° for 6 hours, then diluted with 1000 parts of cold water. Sufficient potassium carbonate is added to insure basicity. The mixture thus obtained is extracted with toluene. The toluene extract is washed with water, dried over anhydrous potassium carbonate, and stripped of solvent by vacuum distillation, affording 1-(2-azidoethyl)-2-methyl-5-nitroimidazole as a yellow oil which is further purified by crystallization from ether. Isolated by filtration, washed with a 1:1 mixture of ether and hexane, and dried in air the purified product melts at 53°-54°. It has the formula ##SPC6##

후처리

  1. customThe mixture thus obtained
  2. extractionis extracted with toluene
  3. extractionThe toluene extract
  4. washis washed with water
  5. dry with materialdried over anhydrous potassium carbonate
  6. distillationstripped of solvent by vacuum distillation

출처 및 근거

ORD 기록
ord-c45319989cf84c249d0752ce9a50e2b3
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03962274

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