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Hydrochloric Acid → 4-((2-(benzyloxy)-4,6-dimethylpyridin-3-yl)methyl)-9-bromo-7-isopropoxy-6-methyl-3,4-dihydrobenzo[f][1,4]oxazepin-5(2H)-one

HRID 577558
ノート
印刷プレビュー

反応式

HRID 577558 の反応式
[CH2:1]([O:8][C:9]1[C:14]([CH2:15][NH:16][CH2:17][CH2:18][O:19][C:20]2[C:30]([Br:31])=[CH:29][C:28]([O:32]S(C)(=O)=O)=[C:27]([CH3:37])[C:21]=2[C:22]([O:24]CC)=O)=[C:13]([CH3:38])[CH:12]=[C:11]([CH3:39])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].Cl.[CH:43](N(CC)C(C)C)([CH3:45])[CH3:44].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(=O)([O-])[O-].[Cs+].[Cs+].IC(C)C>CO.O>[CH2:1]([O:8][C:9]1[C:14]([CH2:15][N:16]2[C:22](=[O:24])[C:21]3[C:27]([CH3:37])=[C:28]([O:32][CH:43]([CH3:45])[CH3:44])[CH:29]=[C:30]([Br:31])[C:20]=3[O:19][CH2:18][CH2:17]2)=[C:13]([CH3:38])[CH:12]=[C:11]([CH3:39])[N:10]=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

10

反応物 7

HCID 313Hydrochloric AcidHCID 6362Isopropyl iodideHCID 10796Cesium carbonateHCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 86723784
Ethyl 2-(2-(((2-(benzyloxy)-4,6-dimethylpyridin-3-yl)methyl)amino)ethoxy)-3-bromo-6-methyl-5-((methylsulfonyl)oxy)benzoate

生成物 1

HCID 867237854-((2-(benzyloxy)-4,6-dimethylpyridin-3-yl)methyl)-9-bromo-7-isopropoxy-6-methyl-3,4-dihydrobenzo[f][1,4]oxazepin-5(2H)-one収率 25,003.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒3 回

反応条件

温度
120 °C

実験手順

To a solution of ethyl 2-(2-(((2-(benzyloxy)-4,6-dimethylpyridin-3-yl)methyl)amino)-ethoxy)-3-bromo-6-methyl-5-((methylsulfonyl)oxy)benzoate (116f, 0.54 g, 0.86 mmol) in methanol (2 mL) was added sodium hydroxide solution (50% in water, 0.73 g, 9.2 mmol). The reaction mixture was heated at 120° C. in the microwave for 1 hour then diluted with water and acidified with concentrated hydrochloric acid to pH ˜4. The resulting precipitate was collected by vacuum filtration then taken up in N,N-dimethylacetamide (5 mL). N,N-diisopropylethyl amine (0.38 mL, 2.2 mmol) and O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HATU, 0.39 g, 1.0 mmol) were added and the reaction was stirred at room temperature overnight. The crude reaction was diluted with water (10 mL) and extracted with dichloromethane (2×15 mL). The combined organic layers were washed with brine (15 mL), dried over magnesium sulfate and concentrated under vacuum. The residue was dissolved in N,N-dimethylacetamide (5 mL) and cesium carbonate (0.51 g, 1.6 mmol) and 2-iodopropane (0.12 mL, 1.2 mmol) were added. The mixture was heated at 75° C. for 1 hour, cooled to room temperature then diluted with water (10 mL) and extracted with ethyl acetate (2×15 mL). The combined organic layers were washed with brine (15 mL), dried over magnesium sulfate, concentrated under vacuum, and purified by column chromatography (30% EtOAc/Heptane) to give 4-((2-(benzyloxy)-4,6-dimethylpyridin-3-yl)methyl)-9-bromo-7-isopropoxy-6-methyl-3,4-dihydrobenzo[f][1,4]oxazepin-5(2H)-one (116 g, 242 mg, 48% yield) as a clear sticky solid.

後処理

  1. filtrationThe resulting precipitate was collected by vacuum filtration
  2. customThe crude reaction
  3. extractionextracted with dichloromethane (2×15 mL)
  4. washThe combined organic layers were washed with brine (15 mL)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum
  7. dissolutionThe residue was dissolved in N,N-dimethylacetamide (5 mL)
  8. temperatureThe mixture was heated at 75° C. for 1 hour
  9. temperaturecooled to room temperature
  10. extractionextracted with ethyl acetate (2×15 mL)
  11. washThe combined organic layers were washed with brine (15 mL)
  12. dry with materialdried over magnesium sulfate
  13. concentrationconcentrated under vacuum
  14. custompurified by column chromatography (30% EtOAc/Heptane)

出典と根拠

ORDレコード
ord-5d67d62296544f6f819c3d965d5d65be
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040515B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート