Hydrochloric Acid → 6-Acetyl-8-cyclopentyl-5-methyl-2-((5-(4-methylpiperazin-1-yl)pyridin-2-yl)amino)-8H-pyrido(2,3-d)pyrimidin-7-one

HRID 586501노트

반응식

HRID 586501 반응식
[CH:1]1([N:6]2[C:11]3[N:12]=[C:13]([NH:16][C:17]4[CH:22]=[CH:21][C:20]([N:23]5[CH2:28][CH2:27][N:26]([CH3:29])[CH2:25][CH2:24]5)=[CH:19][N:18]=4)[N:14]=[CH:15][C:10]=3[C:9]([CH3:30])=[C:8]([C:31]([O:33]CC)=[CH2:32])[C:7]2=[O:36])[CH2:5][CH2:4][CH2:3][CH2:2]1.Cl>C(Cl)(Cl)Cl>[C:31]([C:8]1[C:7](=[O:36])[N:6]([CH:1]2[CH2:5][CH2:4][CH2:3][CH2:2]2)[C:11]2[N:12]=[C:13]([NH:16][C:17]3[CH:22]=[CH:21][C:20]([N:23]4[CH2:24][CH2:25][N:26]([CH3:29])[CH2:27][CH2:28]4)=[CH:19][N:18]=3)[N:14]=[CH:15][C:10]=2[C:9]=1[CH3:30])(=[O:33])[CH3:32]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 102890078-cyclopentyl-6-(1-ethoxy-vinyl)-5-methyl-2-[5-(4-methyl-piperazin-1-yl)-pyridin-2-ylamino]-8H-pyrido[2,3-d]pyrimidin-7-one

생성물 1

HCID 53302986-Acetyl-8-cyclopentyl-5-methyl-2-((5-(4-methylpiperazin-1-yl)pyridin-2-yl)amino)-8H-pyrido(2,3-d)pyrimidin-7-one수율 108.3%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 8-cyclopentyl-6-(1-ethoxy-vinyl)-5-methyl-2-[5-(4-methyl-piperazin-1-yl)-pyridin-2-ylamino]-8H-pyrido[2,3-d]pyrimidin-7-one (237 mg, 0.48 mmol) in chloroform (5 ml) was added hydrogen chloride (2 M ethereal solution, 2.0 ml, 4.0 mmol). The reaction mixture was stirred at RT for 12 h. The solvents were evaporated and the residue was dissolved in ethanol. The ethanol was evaporated to give 6-acetyl-8-cyclopentyl-5-methyl-2-[5-(4-methyl-piperazin-1-yl)-pyridin-2-ylamino]-8H-pyrido[2,3-d]pyrimidin-7-one (239 mg, 0.52 mmol). MS (APCI+) 462 (M+1, 100); 1H NMR δ(400 MHz, DMSOd6) 10.83 (m, 2H), 9.00 (s, 1H), 8.1 (m, 1H), 7.88-7.82 (m, 2H), 5.89-5.80 (m, 1H), 3.88-3.85 (m, 2H), 3.54-3.51 (m, 2H), 3.23-3.11 (m, 4H), 2.83-2.82 (m, 3H), 2.43 (s, 3H), 2.34 (s, 3H), 2.23-2.11 (m, 2H), 1.93 (br, 2H), 1.81-1.77 (m, 2H), 1.60-1.59 (m, 2H); Anal. Calc'd for C25H31N7O2, 2.70 HCl, 1.05 C2H5OH: C, 53.50; H, 6.63; N, 16.12. Found: C, 53.45; H, 6.47; N, 15.85.

후처리

  1. customThe solvents were evaporated
  2. dissolutionthe residue was dissolved in ethanol
  3. customThe ethanol was evaporated

출처 및 근거

ORD 기록
ord-74e2ad5a857445f08a590970a9448949
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06936612B2

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