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

HRID 1362864노트

반응식

HRID 1362864 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9681006cbfe349ed97db402e96736d84
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07884098B2

반응 노트

불러오는 중…