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Potassium Carbonate → 5-chloro-3-(5-(2-(2-hydroxypropan-2-yl)pyrimidin-4-yl)-2-methylphenyl)-2-methyl-6-((2-methylthiazol-4-yl)methoxy)pyrimidin-4(3H)-one

HRID 2172619
ノート
印刷プレビュー

反応式

HRID 2172619 の反応式
[Cl:1][C:2]1[C:3](=[O:28])[N:4]([C:17]2[CH:22]=[C:21]([C:23](=O)[C:24]#[CH:25])[CH:20]=[CH:19][C:18]=2[CH3:27])[C:5]([CH3:16])=[N:6][C:7]=1[O:8][CH2:9][C:10]1[N:11]=[C:12]([CH3:15])[S:13][CH:14]=1.Cl.[OH:30][C:31]([CH3:36])([CH3:35])[C:32]([NH2:34])=[NH:33].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[C:3](=[O:28])[N:4]([C:17]2[CH:22]=[C:21]([C:23]3[CH:24]=[CH:25][N:34]=[C:32]([C:31]([OH:30])([CH3:36])[CH3:35])[N:33]=3)[CH:20]=[CH:19][C:18]=2[CH3:27])[C:5]([CH3:16])=[N:6][C:7]=1[O:8][CH2:9][C:10]1[N:11]=[C:12]([CH3:15])[S:13][CH:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 426142842-Hydroxy-2-methylpropanimidamide hydrochlorideHCID 715815745-chloro-2-methyl-3-(2-methyl-5-propynoyl-phenyl)-6-(2-methyl-thiazol-4-ylmethoxy)-3H-pyrimidin-4-one

生成物 1

HCID 715825025-chloro-3-(5-(2-(2-hydroxypropan-2-yl)pyrimidin-4-yl)-2-methylphenyl)-2-methyl-6-((2-methylthiazol-4-yl)methoxy)pyrimidin-4(3H)-one収率 11.5%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

反応条件

温度
75 °C

実験手順

To a solution of 5-chloro-2-methyl-3-(2-methyl-5-propynoyl-phenyl)-6-(2-methyl-thiazol-4-ylmethoxy)-3H-pyrimidin-4-one from Step C (87 mg, 0.21 mmol) in acetonitrile (2 mL) was added 2-hydroxy-2-methylpropionamidine HCl (44 mg, 0.32 mmol) and potassium carbonate (87 mg, 0.63 mmol) and the slurry was heated at 75° C. for two hours and at ambient temperature for eighteen hours. The reaction was filtered to remove excess salts. The filtrate was concentrated and purified via normal phase chromatography (ethyl acetate/heptane) to provide the title compound as a white solid (12 mg, 11% yield). MS (M+H): 499; 1H NMR (400 MHz, chloroform-d) δ ppm, 1.64 (s, 6H), 2.17 (s, 3H), 2.21 (s, 3H), 2.77 (s, 3H), 5.59-5.68 (m, 2H), 7.26 (s, 1H), 7.55-7.59 (m, 2H), 7.93 (s, 1H), 8.14 (d, J=8.60, 1H), 8.78 (d, J=5.08, 1H).

後処理

  1. filtrationThe reaction was filtered
  2. customto remove excess salts
  3. concentrationThe filtrate was concentrated
  4. custompurified via normal phase chromatography (ethyl acetate/heptane)

出典と根拠

ORDレコード
ord-9b5625de784e4e73b5a88e8129a1ca6c
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09056110B2

反応ノート

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