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Potassium Carbonate → 2-Chloro-4-phenylpyridin-3-amine

HRID 1401116
ノート
印刷プレビュー

反応式

HRID 1401116 の反応式
C(OC(=O)[NH:7][C:8]1[C:9]([Cl:15])=[N:10][CH:11]=[CH:12][C:13]=1I)(C)(C)C.[C:17]1(B(O)O)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>>[Cl:15][C:9]1[C:8]([NH2:7])=[C:13]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:12]=[CH:11][N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 66827Phenylboronic AcidHCID 24229170(2-Chloro-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester

生成物 1

HCID 108220922-Chloro-4-phenylpyridin-3-amine

実験手順

(2-chloro-4-iodo-pyridin-3-yl)-carbamic acid tert-butyl ester a (4.20 g, 11.8 mmol), phenyl boronic acid (1.90 g, 15.6 mmol), potassium carbonate (2.42 g, 17.5 mmol) and tetrakistriphenylphosphine palladium(0) (0.68 g, 0.59 mmol) were weighed into a 20 ml microwave vial. The vial was evacuated, then purged with nitrogen gas 3 times. 16.7 ml dry DMF was added, then 3.3 ml of water, which had been degassed by bubbling nitrogen through it overnight. The vial was then capped and microwaved at 130° C. for 40 minutes. The resulting solution was poured into 250 ml water and extracted with EtOAc (3×50 ml). The combined organics were dried with MgSO4, filtered and concentrated. The resulting oil was adsorbed onto silica gel and purified by flash chromatography (150 g SiO2, 0% to 40% EtOAc in hexanes) to give 2-chloro-3-amino-4-phenyl pyridine b (0.84 g, 4.1 mmol, 35%) and the Boc-protected 2-chloro-3-amino-4-phenyl pyridine c (1.74 g, 5.7 mmol, 48%) as yellow and white solids, respectively.

後処理

  1. customThe vial was evacuated
  2. custompurged with nitrogen gas 3 times
  3. addition16.7 ml dry DMF was added
  4. custom3.3 ml of water, which had been degassed
  5. customby bubbling nitrogen through it overnight
  6. customThe vial was then capped
  7. custommicrowaved at 130° C. for 40 minutes
  8. additionThe resulting solution was poured into 250 ml water
  9. extractionextracted with EtOAc (3×50 ml)
  10. dry with materialThe combined organics were dried with MgSO4
  11. filtrationfiltered
  12. concentrationconcentrated
  13. custompurified by flash chromatography (150 g SiO2, 0% to 40% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-5bea34e9886646218d412df73cc2efd9
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08907092B2

反応ノート

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