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

HRID 34972ノート

反応式

HRID 34972 の反応式
[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]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 212972634-(2-Propyl-3-chloro-4-acetylphenoxy)butane nitrileHCID 178484365HCID 178484365、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7298b72149514b3780afca07e5e83947
出典データセット
uspto-grants-1988_08
特許番号
US04764521

反応ノート

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