Methyl iodide → 2-[2-(4-{[4-Chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl]-1-methyl-5-{[2-(methyloxy)-5-pyrimidinyl]methyl}-4(1H)-pyrimidinone

HRID 706003ノート

反応式

HRID 706003 の反応式
[Cl:1][C:2]1[CH:32]=[CH:31][C:5]([O:6][C:7]2[CH:30]=[CH:29][C:10]([CH2:11][CH2:12][C:13]3[NH:14][CH:15]=[C:16]([CH2:20][C:21]4[CH:22]=[N:23][C:24]([O:27][CH3:28])=[N:25][CH:26]=4)[C:17](=[O:19])[N:18]=3)=[CH:9][CH:8]=2)=[CH:4][C:3]=1[C:33]([F:36])([F:35])[F:34].[CH3:37]CN(C(C)C)C(C)C.CI>ClC(Cl)C>[Cl:1][C:2]1[CH:32]=[CH:31][C:5]([O:6][C:7]2[CH:30]=[CH:29][C:10]([CH2:11][CH2:12][C:13]3[N:14]([CH3:37])[CH:15]=[C:16]([CH2:20][C:21]4[CH:26]=[N:25][C:24]([O:27][CH3:28])=[N:23][CH:22]=4)[C:17](=[O:19])[N:18]=3)=[CH:9][CH:8]=2)=[CH:4][C:3]=1[C:33]([F:34])([F:35])[F:36]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 81531DiisopropylethylamineHCID 178494125HCID 178494125、化合物

生成物 1

HCID 677749402-[2-(4-{[4-Chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl]-1-methyl-5-{[2-(methyloxy)-5-pyrimidinyl]methyl}-4(1H)-pyrimidinone収率 15.81%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

To the solution of 2-(4-(4-chloro-3-(trifluoromethyl)phenoxy)phenethyl)-5-((2-methoxypyrimidin-5-yl)methyl)pyrimidin-4(1H)-one (308 mg, 0.596 mmol) in dichloroethane (8 mL) was added DIPEA (0.208 mL, 1.192 mmol) and MeI (0.045 mL, 0.715 mmol). The reaction mixture was stirred at room temp overnight. Concentration and purification via MDAP then provided the title compound (50 mg, 15.81% yield). LCMS: rt=3.09 min, [M+H+]=531

後処理

  1. concentrationConcentration and purification via MDAP

出典と根拠

ORDレコード
ord-66557ad4474a4708b6f13f39dc431e3a
出典データセット
uspto-grants-2015_11
特許番号
US09174968B2

反応ノート

読み込み中…