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Sodium Carbonate → 5-(2-Chloro-pyrimidin-4-yl)-2-pyrrolidin-1-yl-benzonitrile

HRID 1852407
ノート
印刷プレビュー

反応式

HRID 1852407 の反応式
[N:1]1([C:6]2[CH:13]=[CH:12][C:11](B3OC(C)(C)C(C)(C)O3)=[CH:10][C:7]=2[C:8]#[N:9])[CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:23][C:24]1[N:29]=[C:28](Cl)[CH:27]=[CH:26][N:25]=1.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:23][C:24]1[N:29]=[C:28]([C:11]2[CH:12]=[CH:13][C:6]([N:1]3[CH2:2][CH2:3][CH2:4][CH2:5]3)=[C:7]([CH:10]=2)[C:8]#[N:9])[CH:27]=[CH:26][N:25]=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

6

反応物 3

HCID 10340Sodium CarbonateHCID 775312,4-DichloropyrimidineHCID 666923072-(Pyrrolidin-1-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile

生成物 1

HCID 866983255-(2-Chloro-pyrimidin-4-yl)-2-pyrrolidin-1-yl-benzonitrile収率 381.1%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物
触媒
HCID 218864351,4-Dioxane--water (1/1)溶媒

反応条件

温度
100 °C

実験手順

Pyrrolidin-1-yl-5-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzonitrile (200 mg, 0.67 mmol), 2,4-dichloropyrimidine (120 mg, 0.81 mmol), tetrakis(triphenylphosphine)palladium(0) (78 mg, 0.07 mmol, 10 mol %) and sodium carbonate (213 mg, 2.01 mmol) were diluted with 1:1 1,4-dioxane-H2O (4.0 mL). The mixture was then heated at 100° C. in the microwave (300 W, stirring) for 10 minutes. The reaction was repeated four more times. The reaction mixtures were combined and the solvents evaporated in vacuo (Genevac™). The residue was partitioned between DCM (150 mL) and H2O (50 mL). The organic phase was washed with water (50 mL) and saturated brine solution (75 mL). The organic phase was then dried (MgSO4), filtered and the solvent evaporated in vacuo. The crude product was purified by column chromatography (40-63 mesh silica gel, 70% isohexane-EtOAc) to provide the title compound as a yellow solid (727 mg, 76%); LC-MS, Rt=2.80 min (MeOH-FA method), m/z 285, 287 (MH+).

後処理

  1. customThe reaction mixtures
  2. customthe solvents evaporated in vacuo (Genevac™)
  3. customThe residue was partitioned between DCM (150 mL) and H2O (50 mL)
  4. washThe organic phase was washed with water (50 mL) and saturated brine solution (75 mL)
  5. dry with materialThe organic phase was then dried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent evaporated in vacuo
  8. customThe crude product was purified by column chromatography (40-63 mesh silica gel, 70% isohexane-EtOAc)

出典と根拠

ORDレコード
ord-25f1dc9559af4adca23c16b6708af903
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962609B2

反応ノート

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