1H-Indazol-6-amine → 2-[(4-t-Butylbenzoyl)amino]-N-(6-indazolyl)-5-nitrobenzamide

HRID 842384

반응식

HRID 842384 반응식
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[N:12]=[C:11]([C:13]3[CH:18]=[CH:17][C:16]([C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:15][CH:14]=3)[O:10][C:9](=[O:23])[C:8]=2[CH:24]=1)([O-:3])=[O:2].[NH2:25][C:26]1[CH:34]=[C:33]2[C:29]([CH:30]=[N:31][NH:32]2)=[CH:28][CH:27]=1>C1(C)C=CC=CC=1>[C:19]([C:16]1[CH:17]=[CH:18][C:13]([C:11]([NH:12][C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:24][C:8]=2[C:9]([NH:25][C:26]2[CH:34]=[C:33]3[C:29]([CH:30]=[N:31][NH:32]3)=[CH:28][CH:27]=2)=[O:23])=[O:10])=[CH:14][CH:15]=1)([CH3:20])([CH3:22])[CH3:21]

참가 물질

4

반응물 2

HCID 814231H-Indazol-6-amineHCID 3855992-(4-Tert-butylphenyl)-6-nitro-3,1-benzoxazin-4-one

생성물 1

HCID 183731892-[(4-t-Butylbenzoyl)amino]-N-(6-indazolyl)-5-nitrobenzamide수율 42.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a stirring solution of 6-nitro-2-[4-t-butylphenyl]-4H-3,1-benzoxazin-4-one (1.5 g, 4.62 mmol) in toluene (25 mL) was added 6-aminoindazole (560 mg, 4.2 mmol) and the solution was heated to reflux. After about 24 h, the solution was cooled, filtered and the solid was washed with diethyl ether. The product was then chromatographed over silica gel, eluting with 25% ethyl acetate/hexanes. The product containing fractions were combined and concentrated in vacuo to give 810 mg (42%) of pale yellow solid.

후처리

  1. temperaturethe solution was heated to reflux
  2. temperaturethe solution was cooled
  3. filtrationfiltered
  4. washthe solid was washed with diethyl ether
  5. customThe product was then chromatographed over silica gel
  6. washeluting with 25% ethyl acetate/hexanes
  7. additionThe product containing fractions
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-afe226187cf645d8a41ba8893b54973c
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06372759B1

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