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Dichloromethane → 5-(4-Morpholino-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidin-2-yl)pyrimidin-2-amine

HRID 528451
ノート
印刷プレビュー

反応式

HRID 528451 の反応式
Cl[C:2]1[N:3]=[C:4]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[C:5]2[O:11][CH2:10][CH2:9][O:8][C:6]=2[N:7]=1.CC1(C)C(C)(C)OB([C:26]2[CH:27]=[N:28][C:29]([NH2:32])=[N:30][CH:31]=2)O1.C(Cl)Cl.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.O>[O:15]1[CH2:16][CH2:17][N:12]([C:4]2[C:5]3[O:11][CH2:10][CH2:9][O:8][C:6]=3[N:7]=[C:2]([C:26]3[CH:27]=[N:28][C:29]([NH2:32])=[N:30][CH:31]=3)[N:3]=2)[CH2:13][CH2:14]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

7

反応物 4

HCID 6344Dichloromethane2 回HCID 10796Cesium carbonateHCID 177502122-Aminopyrimidine-5-boronic acid, pinacol ester2 回HCID 867117372-Chloro-4-morpholin-4-yl-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidine

生成物 1

HCID 867117385-(4-Morpholino-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidin-2-yl)pyrimidin-2-amine

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-chloro-4-morpholin-4-yl-6,7-dihydro-[1,4]dioxino[2,3-d]pyrimidine (114 mg, 0.44 mmol), 5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyrimidin-2-ylamine (196 mg, 0.88 mmol), PdCl2dppf.DCM (36 mg, 0.04 mmol) and cesium carbonate (430 mg, 1.32 mmol) in dioxane (5 mL) and water (0.5 mL) was degassed and then heated at 100° C. for 2 hours. Further 5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-pyrimidin-2-ylamine (100 mg, 0.44 mmol), PdCl2dppf.DCM (36 mg, 0.04 mmol) were added and the mixture heated at 100° C. for a further 2 hours. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic extracts were dried (Na2SO4) and concentrated in vacuo. The resulting residue was loaded onto an Isolute® SCX-2 cartridge which was washed with methanol and the product eluted with 2M ammonia in methanol. The basic fractions were combined and concentrated in vacuo. The resulting residue was purified by column chromatography (SiO2, gradient 0-10% methanol in DCM) then triturated with diethyl ether affording 101 (37 mg, 27%). LCMS: RT=2.75 min, [M+H]+=317. 1H NMR (400 MHz, DMSO): δ 8.90 (2H, s), 7.01 (2H, s), 4.42-4.36 (2H, m), 4.25-4.18 (2H, m), 3.70 (8H, s).

後処理

  1. temperaturethe mixture heated at 100° C. for a further 2 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic extracts were dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. washwas washed with methanol
  6. washthe product eluted with 2M ammonia in methanol
  7. concentrationconcentrated in vacuo
  8. customThe resulting residue was purified by column chromatography (SiO2, gradient 0-10% methanol in DCM)
  9. customthen triturated with diethyl ether affording 101 (37 mg, 27%)

出典と根拠

ORDレコード
ord-92d2dcec0a0c4b3d9c9bb5b6aa66f9a7
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09346817B2

反応ノート

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