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

HRID 842384

反応式

HRID 842384 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-afe226187cf645d8a41ba8893b54973c
出典データセット
uspto-grants-2002_04
特許番号
US06372759B1

関連ノート

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