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Dimethylformamide → 9-Phenyl-2-(3-pyridyl)purine-6-carboxamide

HRID 2427953
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HRID 2427953 반응식
[NH2:1][C:2]1[C:3]([C:21]([O:23]C)=O)=[N:4][C:5]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[N:6]C=1NC1C=CC=CC=1.NC1C(C(OC)=O)=NC(Cl)=NC=1N[C:33]1[CH:38]=[CH:37]C=[CH:35][CH:34]=1.C([Sn](CCCC)(CCCC)C1C=[N:51]C=CC=1)CCC.[CH3:63][N:64]([CH:66]=O)[CH3:65]>>[C:65]1([N:64]2[CH:66]=[N:1][C:2]3[C:63]2=[N:6][C:5]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[N:4][C:3]=3[C:21]([NH2:51])=[O:23])[CH:37]=[CH:38][CH:33]=[CH:34][CH:35]=1
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참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 34838483-(Tributylstannyl)pyridineHCID 57474558Methyl 5-amino-2-chloro-6-(phenylamino)pyrimidine-4-carboxylateHCID 57474559Methyl 5-amino-6-(phenylamino)-2-(3-pyridyl)pyrimidine-4-carboxylate

생성물 1

HCID 249378619-Phenyl-2-(3-pyridyl)purine-6-carboxamide수율 57%

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온도
120 °C

실험 절차

Methyl 5-amino-6-(phenylamino)-2-(3-pyridyl)pyrimidine-4-carboxylate. To a solution of methyl 5-amino-2-chloro-6-(phenylamino)pyrimidine-4-carboxylate (0.189 g, 0.68 mmol) in anhydrous DMF (3.5 mL) was added 3-(tributylstannyl)pyridine (1.252 g, 3.4 mmol), and dichlorobis(triphenylphosphine) palladium(II) (0.239 g, 0.34 mmol). The solution was purged with nitrogen then heated in an Emrys Optimizer microwave reactor for 30 minutes at 120° C. The volatiles were evaporated and the resulting residue was purified using chromatography on a normal phase silica gel column (1-10% methanol in dichloromethane). Fractions containing product were combined and the solvent evaporated. The material was re-purified using reverse-phase preparatory HPLC (30-80% acetonitrile+0.1% TFA in H2O+0.1% TFA, over 30 minutes). Fractions containing the desired material were combined and concentrated under reduced pressure before being passed through a Strata-XC ion exchange column with water, methanol, and 5% ammonium hydroxide in methanol. The resulting solid was dried under high vacuum at 60° C. to afford the title compound (0.125 g, 0.389 mmol, 57% yield). MS (ESI) m/z 322.4 [M+1]+.

후처리

  1. customThe solution was purged with nitrogen
  2. customThe volatiles were evaporated
  3. customthe resulting residue was purified
  4. additionFractions containing product
  5. customthe solvent evaporated
  6. customThe material was re-purified
  7. customreverse-phase preparatory HPLC (30-80% acetonitrile+0.1% TFA in H2O+0.1% TFA, over 30 minutes)
  8. additionFractions containing the desired material
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting solid was dried under high vacuum at 60° C.

출처 및 근거

ORD 기록
ord-d019e5f8a62b495694e8bfa0aa2e865f
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07968556B2

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