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Potassium Phosphate, Tribasic → 5-Benzylpyridin-2-amine

HRID 2075269
ノート
印刷プレビュー

反応式

HRID 2075269 の反応式
[CH2:1](B1C2CCCC1CCC2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.I[C:18]1[CH:19]=[CH:20][C:21]([NH2:24])=[N:22][CH:23]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].CC(C1C=C(C(C)C)C(C2C=CC=CC=2P(C2CCCCC2)C2CCCCC2)=C(C(C)C)C=1)C>O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH2:1]([C:18]1[CH:19]=[CH:20][C:21]([NH2:24])=[N:22][CH:23]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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 62657Potassium Phosphate, TribasicHCID 885792-Pyridinamine, 5-iodo-HCID 41509249-Benzyl-9-borabicyclo(3.3.1)nonaneHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl

生成物 1

HCID 134300735-Benzylpyridin-2-amine

試薬・触媒・溶媒 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

9-Benzyl-9-bora-bicyclo[3.3.1]nonane (0.5M solution in THF, 12727 μL, 6363 μmol) was added to a mixture of 5-iodopyridin-2-amine (700 mg, 3182 μmol), potassium phosphate (2026 mg, 9545 μmol), Pd2 dba3 (58 mg, 64 μmol), and X-Phos (61 mg, 127 μmol) suspended in H2O (1 mL) in a sealable reaction vial. The vial was flushed with argon gas and then sealed and heated (microwave) at 120° C. for 30 min. The crude mixture was diluted with EtOAc, and the resulting solution was sequentially washed with 1M NaOH and brine. The organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was taken up in MeOH (5 mL), concentrated aqueous HCl (0.30 mL) was added, and the resulting solution was stirred 10 min. Solid NaOH (120 mg) was then added, and the resulting solution was concentrated onto silica gel. Chromatographic purification of the product (ISCO, 12 g, 0-10% MeOH/CH2Cl2) furnished 5-benzylpyridin-2-amine as a yellow solid. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 7.95 (s, 1H), 7.28 (t, J=7.5 Hz, 2H), 7.23 (d, J=11.0 Hz, 2H), 7.17 (t, J=8.5 Hz, 2H), 6.44 (d, J=8.5 Hz, 1H), 4.34 (s, 2H), 3.80-3.86 (m, 2H).

後処理

  1. customThe vial was flushed with argon gas
  2. customsealed
  3. additionThe crude mixture was diluted with EtOAc
  4. washthe resulting solution was sequentially washed with 1M NaOH and brine
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. additionconcentrated aqueous HCl (0.30 mL) was added
  8. additionSolid NaOH (120 mg) was then added
  9. concentrationthe resulting solution was concentrated onto silica gel
  10. customChromatographic purification of the product (ISCO, 12 g, 0-10% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-e80af44b8616444489db23086ab2d17c
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07919519B2

反応ノート

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