Dimethylformamide → 5-[4-(2-Propyl-3-chloro-4-acetylphenoxy)butyl]-tetrazole

HRID 34972노트

반응식

HRID 34972 반응식
[CH2:1]([C:4]1[C:15]([Cl:16])=[C:14]([C:17](=[O:19])[CH3:18])[CH:13]=[CH:12][C:5]=1[O:6][CH2:7][CH2:8][CH2:9][C:10]#N)[CH2:2][CH3:3].[N-:20]=[N+:21]=[N-:22].[CH3:23][N:24](C)C(=[NH2+])N(C)C.CN(C)C=O.C(OCC)(=O)C>O>[CH2:1]([C:4]1[C:15]([Cl:16])=[C:14]([C:17](=[O:19])[CH3:18])[CH:13]=[CH:12][C:5]=1[O:6][CH2:7][CH2:8][CH2:9][CH2:10][C:23]1[NH:24][N:22]=[N:21][N:20]=1)[CH2:2][CH3:3]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 212972634-(2-Propyl-3-chloro-4-acetylphenoxy)butane nitrileHCID 178484365HCID 178484365, 화합물

생성물 1

HCID 1784396765-[4-(2-Propyl-3-chloro-4-acetylphenoxy)butyl]-tetrazole

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 0.5 g. of 4-(2-propyl-3- chloro-4-acetylphenoxy)butane nitrile and 1.3 g. of tetramethylguanidinium azide in 3 ml. of dimethylformamide was heated overnight at 125° C. The reaction was cooled, ethyl acetate and water were added, and the layers were separated. Water was added to the ethyl acetate layer, the water layer was acidified, and the layers were separated. The ethyl acetate was dried and evaporated to dryness. The residue was purified by chromatography to give the desired title product. NMR.

후처리

  1. temperatureThe reaction was cooled
  2. customthe layers were separated
  3. additionWater was added to the ethyl acetate layer
  4. customthe layers were separated
  5. dry with materialThe ethyl acetate was dried
  6. customevaporated to dryness
  7. customThe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-7298b72149514b3780afca07e5e83947
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04764521

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