2-Amino-3-(trifluoromethyl)benzonitrile → 3-Amino-6-(trifluoromethyl)-1H-indazole

HRID 1283705

반응식

HRID 1283705 반응식
[C:1]([C:3]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:4]=1[NH2:5])#[N:2].[N:14]([O-])=O.[Na+]>Cl>[NH2:2][C:1]1[C:3]2[C:4](=[CH:6][C:7]([C:10]([F:11])([F:12])[F:13])=[CH:8][CH:9]=2)[NH:5][N:14]=1

참가 물질

4

반응물 2

HCID 134390282-Amino-3-(trifluoromethyl)benzonitrileHCID 23668193Sodium Nitrite

생성물 1

HCID 8179093-Amino-6-(trifluoromethyl)-1H-indazole

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

To a mixture of 18.6 g. of 2-cyano-5-trifluoromethylaniline and 120 ml. of concentrated hydrochloric acid is added dropwise 8.0 g. of sodium nitrite in aqueous solution. The resulting diazo solution is added dropwise to 152 g. of stannous chloride in concentrated hydrochloric acid at 0° C. After allowing the mixture to stand for several hours at 0° C., it is filtered. The solid is treated with boiling water and the solution is made alkaline. The precipitate is recrystallized from benzene to give 3-amino-6-trifluoromethylindazole, M.P. 168°-169° C.

후처리

  1. additionTo a mixture of 18.6 g
  2. customat 0° C
  3. waitto stand for several hours at 0° C.
  4. filtrationit is filtered
  5. additionThe solid is treated with boiling water
  6. customThe precipitate is recrystallized from benzene

출처 및 근거

ORD 기록
ord-826482f045394eba86ee79ed73efde15
출처 데이터셋
uspto-grants-1976_08
특허 번호
USRE028939

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