Hydrazoic acid → HCID 178420316、化合物

HRID 261802

反応式

HRID 261802 の反応式
[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH:13]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[NH4+].[N-]=[N+]=[N-].[Na+].C(N1C=CN=C1C#N)C1C=CC=CC=1.N=[N+]=[N-].[NH:38]1C=[N:41][N:40]=[N:39]1>CN(C)C=O.O>[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[C:13]1[NH:41][N:40]=[N:39][N:38]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

9

反応物 6

HCID 24530Hydrazoic acidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 1390821-benzyl-1H-imidazole-2-carbaldehydeHCID 110304751H-Imidazole-2-carbonitrile, 1-(phenylmethyl)-HCID 178418441HCID 178418441、化合物

生成物 1

HCID 178420316HCID 178420316、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Obtained by reacting 9.3 g (0.05 mol) of 1-benzyl-2-formylimidazole (see Liebigs Ann. Chem. 718 (1968) pp. 249-259) with 8.0 g (0.15 mol) of ammonium chloride and 9.8 g (0.15 mol) of sodium azide in 50 ml of dimethylformamide at 120°-130° C. The isolation of the 1-benzyl-2-cyanoimidazole intermediate (obtained by Schmidt-rearrangement) may be omitted, since this compound adds excess hydrazoic acid to the tetrazole in situ. After 20 hours, it is cooled, and 500 ml of water are added, the precipitate formed filtered off and recrystallised several times from dimethylformamide. M.p. 274°-275° C.

後処理

  1. customObtained
  2. customat 120°-130° C
  3. temperatureit is cooled
  4. customthe precipitate formed
  5. filtrationfiltered off
  6. customrecrystallised several times from dimethylformamide

出典と根拠

ORDレコード
ord-faced8bfa88b4593be37b6ecae11b106
出典データセット
uspto-grants-1979_05
特許番号
US04152440

関連ノート

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