Hydrazoic acid → HCID 178420316, 화합물

HRID 261802

반응식

HRID 261802 반응식
[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

참가 물질

9

반응물 6

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

생성물 1

HCID 178420316HCID 178420316, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-faced8bfa88b4593be37b6ecae11b106
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04152440

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