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Potassium Phosphate, Tribasic → HCID 86664223、化合物

HRID 1184484
ノート
印刷プレビュー

反応式

HRID 1184484 の反応式
P([O-])([O-])([O-])=O.[K+].[K+].[K+].[CH2:9]([B-](F)(F)F)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[K+].Cl[C:22]1[C:27]2[O:28][CH:29]([CH3:33])[C:30](=[O:32])[NH:31][C:26]=2[CH:25]=[C:24]([CH:34]=[O:35])[CH:23]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC(C)C)=CC=CC=2OC(C)C)CCCCC1>C1(C)C=CC=CC=1.O.CC(O)C>[CH2:9]([C:22]1[C:27]2[O:28][CH:29]([CH3:33])[C:30](=[O:32])[NH:31][C:26]=2[CH:25]=[C:24]([CH:34]=[O:35])[CH:23]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=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

8

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 162179852-Dicyclohexylphosphino-2',6'-diisopropoxybiphenylHCID 23692459Potassium benzyltrifluoroboranuideHCID 866642218-Chloro-2-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde

生成物 1

HCID 86664223HCID 86664223、化合物収率 28.2%

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回
HCID 1140Toluene溶媒
HCID 3776Isopropanol溶媒

反応条件

温度
115 °C

実験手順

To a suspension of potassium phosphate, tribasic (0.564 g, 2.66 mmol), potassium benzyltrifluoroborate (0.263 g, 1.330 mmol), 8-chloro-2-methyl-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-carbaldehyde 15 (0.2 g, 0.886 mmol) in toluene (Ratio: 5.00, 20 mL) and water (Ratio: 1.000, 4.0 mL) was added PdOAc2 (0.015 g, 0.066 mmol) and dicyclohexyl(2′,6′-diisopropoxybiphenyl-2-yl)phosphine (0.062 g, 0.133 mmol) at 23° C. The reaction was stirred at 115° C. for 20 hr. The reaction mixture was poured into water (2 mL) and extracted with Et2O (3×5 mL). The organic layer was dried over Na2SO4, filtered, and the organic phase stripped to dryness via rotary evaporation. The resulting crude material was reconstituted in DCM (1.0 mL) and purified via medium pressure chromatography using a gradient eluant of 1-5% MeOH:DCM. The appropriate fractions were combined and solvent was removed via rotary evaporation. The late eluting fractions were dried in vacuo to provide a yellow solid. The yellow solid was re-suspended in IPA (1.0 mL), heated at reflux to furnish a solution, cooled to room temperature, filtered, rinsed with IPA, and dried in vacuo to provide the title compound as an off-white solid (0.0704 g, 0.250 mmol, 28.2% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.36 (d, J=6.82 Hz, 3H) 3.98 (s, 2H) 4.75-4.81 (m, 1H) 7.16-7.32 (m, 6H) 7.45 (d, J=2.02 Hz, 1H) 9.80 (s, 1H) 10.93 (s, 1H). ESI-MS: m/z 282.2 (M+H)+. mp=163.2-166.1° C.

後処理

  1. additionwas added
  2. customat 23° C
  3. extractionextracted with Et2O (3×5 mL)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customthe organic phase stripped to dryness via rotary evaporation
  7. custompurified via medium pressure chromatography
  8. customsolvent was removed via rotary evaporation
  9. washThe late eluting fractions
  10. customwere dried in vacuo
  11. customto provide a yellow solid
  12. temperatureheated
  13. temperatureat reflux
  14. customto furnish a solution
  15. temperaturecooled to room temperature
  16. filtrationfiltered
  17. washrinsed with IPA
  18. customdried in vacuo

出典と根拠

ORDレコード
ord-70fc821f69d74a2dbf7b00581f7e2830
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08669249B2

反応ノート

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