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Potassium Iodide → 4-Amino-8-[1-(3-bromo-5-chloro-2-methoxy-4-methylphenyl)ethyl]pyrido[2,3-d]pyrimidin-5(8H)-one

HRID 1499713
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HRID 1499713 반응식
[NH2:1][C:2]1[C:3]2[C:11](=[O:12])[CH:10]=[CH:9][NH:8][C:4]=2[N:5]=[CH:6][N:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[K+].[Br:21][C:22]1[C:23]([CH3:34])=[C:24]([Cl:33])[CH:25]=[C:26]([CH:30](Cl)[CH3:31])[C:27]=1[O:28][CH3:29]>CN(C)C=O.O.C(OCC)(=O)C>[NH2:1][C:2]1[C:3]2[C:11](=[O:12])[CH:10]=[CH:9][N:8]([CH:30]([C:26]3[CH:25]=[C:24]([Cl:33])[C:23]([CH3:34])=[C:22]([Br:21])[C:27]=3[O:28][CH3:29])[CH3:31])[C:4]=2[N:5]=[CH:6][N:7]=1
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참가 물질

8

반응물 4

HCID 4875Potassium IodideHCID 10796Cesium carbonateHCID 57067884-aminopyrido[2,3-d]pyrimidin-5(8H)-oneHCID 866776443-Bromo-1-chloro-5-(1-chloroethyl)-4-methoxy-2-methylbenzene

생성물 1

HCID 866776524-Amino-8-[1-(3-bromo-5-chloro-2-methoxy-4-methylphenyl)ethyl]pyrido[2,3-d]pyrimidin-5(8H)-one

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

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온도
140 °C

실험 절차

To a mixture of 4-aminopyrido[2,3-d]pyrimidin-5(8H)-one (0.80 g, 4.9 mmol), cesium carbonate (2.4 g, 7.3 mmol) and potassium iodide (82 mg, 0.49 mmol) in N,N-dimethylformamide (20 mL) was added 3-bromo-1-chloro-5-(1-chloroethyl)-4-methoxy-2-methylbenzene (1.47 g, 4.93 mmol) and the mixture was stirred at 140° C. for 1 hour. The mixture was diluted with water and ethyl acetate. The precipitate was collected and dried to give the desired compound. LCMS calculated for C17H17BrClN4O2 (M+H)+: m/z=423.0; Found: 423.0.

후처리

  1. customThe precipitate was collected
  2. customdried

출처 및 근거

ORD 기록
ord-982214d31d01418e9ced8fb219f70fae
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09199982B2

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