Isobutylamine → N1-(1H-5-Indazolyl)-N4-isobutyl-1,4-cyclohexanediamine

HRID 1352170

反応式

HRID 1352170 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([NH:10][CH:11]3[CH2:16][CH2:15][C:14](=O)[CH2:13][CH2:12]3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[CH2:18]([NH2:22])[CH:19]([CH3:21])[CH3:20].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].Cl.CO>CO>[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([NH:10][CH:11]3[CH2:16][CH2:15][CH:14]([NH:22][CH2:18][CH:19]([CH3:21])[CH3:20])[CH2:13][CH2:12]3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1

参加物

6

反応物 4

HCID 6558IsobutylamineHCID 5049666Sodium triacetoxyborohydrideHCID 178382714-(1H-5-Indazolylamino)-1-cyclohexanone2 回HCID 21893726Hydrochloride methanol

生成物 1

HCID 17838119N1-(1H-5-Indazolyl)-N4-isobutyl-1,4-cyclohexanediamine収率 11.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-(1H-5-Indazolylamino)-1-cyclohexanone (intermediate 3) (57 mg) and isobutylamine (37 mg) were dissolved in methanol (1 ml), and sodium triacetoxyborohydride (105 mg) was added by portions to the solution at room temperature. The reaction mixture was stirred at room temperature for 18 hr. Hydrochloric acid-methanol was then added thereto, and the reaction mixture was stirred and was then concentrated. The residue was purified by HPLC [0.5% aqueous trifluoroacetic acid solution/acetonitrile] to give an anti-form compound (8 mg) and a syn-form compound (6 mg).

後処理

  1. stirringthe reaction mixture was stirred
  2. concentrationwas then concentrated
  3. customThe residue was purified by HPLC [0.5% aqueous trifluoroacetic acid solution/acetonitrile]

出典と根拠

ORDレコード
ord-b5c4f08c936746c38f6b5276c2bd6094
出典データセット
uspto-grants-2007_05
特許番号
US07217722B2

関連ノート

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