Hydrochloric Acid → N-(1-methylethyl)-2-[(5-methyl-2-{[3-(4-methyl-2-oxo-1-piperazinyl)phenyl]amino}-4-pyrimidinyl)amino]benzamide

HRID 1362864

反応式

HRID 1362864 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:20]=[CH:19][CH:18]=[CH:17][C:10]=2[C:11]([NH:13][CH:14]([CH3:16])[CH3:15])=[O:12])[C:5]([CH3:21])=[CH:4][N:3]=1.[NH2:22][C:23]1[CH:24]=[C:25]([N:29]2[CH2:34][CH2:33][N:32]([CH3:35])[CH2:31][C:30]2=[O:36])[CH:26]=[CH:27][CH:28]=1.Cl>C(O)(C)C>[CH3:15][CH:14]([NH:13][C:11](=[O:12])[C:10]1[CH:17]=[CH:18][CH:19]=[CH:20][C:9]=1[NH:8][C:6]1[C:5]([CH3:21])=[CH:4][N:3]=[C:2]([NH:22][C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([N:29]3[CH2:34][CH2:33][N:32]([CH3:35])[CH2:31][C:30]3=[O:36])[CH:24]=2)[N:7]=1)[CH3:16]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 579741721-(3-Aminophenyl)-4-methylpiperazin-2-oneHCID 579742052-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide

生成物 1

HCID 24864097N-(1-methylethyl)-2-[(5-methyl-2-{[3-(4-methyl-2-oxo-1-piperazinyl)phenyl]amino}-4-pyrimidinyl)amino]benzamide収率 27.1%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

2-[(2-Chloro-5-methyl-4-pyrimidinyl)amino]-N-(1-methylethyl)benzamide (103 mg, 0.337 mmol) and 1-(3-aminophenyl)-4-methyl-2-piperazinone (68.8 mg, 0.335 mmol) were stirred at 95° C. overnight in isopropanol (10 mL) with 12 N HCl (0.056 mL, 0.673 mmol). The reaction was cooled to room temperature and the solid was filtered off and washed with isopropanol. The solid was chromatographed using reverse phase HPLC eluting with 5-30% acetonitrile containing 0.1% formic acid to give a white solid (43 mg, 27%) after lyophilization of the combined HPLC fractions. MS: M(C26H31N7O2)=473.57, (M+H)+=473.8.

後処理

  1. filtrationthe solid was filtered off
  2. washwashed with isopropanol
  3. customThe solid was chromatographed
  4. washeluting with 5-30% acetonitrile containing 0.1% formic acid

出典と根拠

ORDレコード
ord-9681006cbfe349ed97db402e96736d84
出典データセット
uspto-grants-2011_02
特許番号
US07884098B2

関連ノート

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