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Benzyl Bromide → HCID 67353995、化合物

HRID 1846172
ノート
印刷プレビュー

反応式

HRID 1846172 の反応式
Br[C:2]1[C:3]([CH3:16])=[N:4][C:5]([N:9]2[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]2[CH3:15])=[N:6][C:7]=1[CH3:8].C(P(C(C)(C)C)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:28]1C(C(C)C)=CC(C(C)C)=CC=1C(C)C)(C)(C)C.[OH-:47].[K+].C(Br)C1C=CC=CC=1.[H-].[Na+]>O1CCOCC1.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].O>[CH2:28]([O:47][C:2]1[C:3]([CH3:16])=[N:4][C:5]([N:9]2[C:13]([CH3:14])=[CH:12][CH:11]=[C:10]2[CH3:15])=[N:6][C:7]=1[CH3:8])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:22]=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

9

反応物 5

HCID 7498Benzyl BromideHCID 14797Potassium HydroxideHCID 24758Sodium hydrideHCID 11618717Di-tert-butyl(2',4',6'-tris(propan-2-yl)-(1,1'-biphenyl)-2-yl)phosphaneHCID 67354708HCID 67354708、化合物

生成物 1

HCID 67353995HCID 67353995、化合物

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

To a stirred solution containing 4.87 g (17.4 mmol) of 5-bromo-2-(2,5-dimethyl-1H-pyrrol-1-yl)-4,6-dimethylpyrimidine in 50 mL of 1:1 dioxane-degassed water was added 632 mg (0.69 mmol) of Pd2dba3 followed by 293 mg (0.69 mmol) of 2-di-tert-butylphosphino-2′,4′,6′-triisopropylbiphenyl (L1) and 2.92 g (52.1 mmol) of KOH. The reaction mixture was stirred at 100° C. for 3 h. The cooled reaction mixture was poured into 200 mL of water and extracted with 100 mL of ethyl acetate. The aqueous layer was acidified with HCl (pH 2-3) and then extracted with two 150-mL portions of ethyl acetate. The combined organic layer was washed with 150 mL of brine, dried (MgSO4) and concentrated under diminished pressure. The residue was dissolved in 50 mL of anhydrous THF and treated with 3.10 mL (26.0 mmol) of benzyl bromide followed by 1.40 g (34.8 mmol) of a 60% suspension of NaH in mineral oil. The reaction mixture was stirred at 23° C. for 48 h. The reaction mixture was quenched with satd aq sodium bicarbonate and poured into 150 mL of water and extracted with two 150-mL portions of ether. The combined organic layer was washed with 150 mL of brine, dried (MgSO4) and concentrated under diminished pressure. The residue was purified by chromatography on a silica gel column (20×6 cm). Elution with 9:1 hexanes-ethyl acetate afforded the expected product as a light yellow oil: yield 4.09 g (76%); silica gel TLC Rf 0.6 (6:1 hexanes-ethyl acetate); 1H NMR (CDCl3) δ2.29 (s, 6H), 2.47 (s, 6H), 4.92 (s, 2H), 5.86 (s, 2H) and 7.42 (m, 5H); 13C NMR (CDCl3) δ 14.1, 14.1, 19.1, 19.1, 75.3, 107.9, 107.9, 128.3, 128.6, 128.6, 129.0, 129.0, 129.2, 129.2, 136.0, 147.7, 152.3, 152.3 and 161.6; mass spectrum (APCI), m/z 307.1675 (M)+ (C19H21N3O requires 307.1685).

後処理

  1. customdegassed water
  2. customThe cooled reaction mixture
  3. extractionextracted with 100 mL of ethyl acetate
  4. extractionextracted with two 150-mL portions of ethyl acetate
  5. washThe combined organic layer was washed with 150 mL of brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under diminished pressure
  8. dissolutionThe residue was dissolved in 50 mL of anhydrous THF
  9. stirringThe reaction mixture was stirred at 23° C. for 48 h
  10. customThe reaction mixture was quenched with satd aq sodium bicarbonate
  11. additionpoured into 150 mL of water
  12. extractionextracted with two 150-mL portions of ether
  13. washThe combined organic layer was washed with 150 mL of brine
  14. dry with materialdried (MgSO4)
  15. concentrationconcentrated under diminished pressure
  16. customThe residue was purified by chromatography on a silica gel column (20×6 cm)
  17. washElution with 9:1 hexanes-ethyl acetate

出典と根拠

ORDレコード
ord-7f57fcdc530a4ad88e1efbd2c31c1aa8
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952025B2

反応ノート

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