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Potassium Carbonate → HCID 86684921、化合物

HRID 2402905
ノート
印刷プレビュー

反応式

HRID 2402905 の反応式
Br[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH3:8])[CH:3]=1.C([O-])(=O)C.[K+].CC1(C)C(C)(C)OB(B2OC(C)(C)C(C)(C)O2)O1.Br[C:33]1[CH:38]=[CH:37][C:36]([S:39][CH2:40][CH2:41][C:42]([NH2:44])=[O:43])=[C:35]([C:45]([F:48])([F:47])[F:46])[CH:34]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].O>[CH3:8][C:4]1[CH:3]=[C:2]([C:33]2[CH:38]=[CH:37][C:36]([S:39][CH2:40][CH2:41][C:42]([NH2:44])=[O:43])=[C:35]([C:45]([F:47])([F:48])[F:46])[CH:34]=2)[CH:7]=[CH:6][N:5]=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 11430Potassium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 27628354-Bromo-2-methylpyridineHCID 86684910HCID 86684910、化合物

生成物 1

HCID 86684921HCID 86684921、化合物収率 71%

試薬・触媒・溶媒 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
80 °C

実験手順

4-Bromo-2-methylpyridine (6.0 g, 34.9 mmol) was dissolved in dimethylformamide (60 mL) before potassium acetate (10.0 g, 102 mmol) and 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (10 g, 39.4 mmol) were added at room temperature. The solution was degassed and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (400 mg, 547 mol) was added. The brown reaction mixture was stirred for 22 h at 80° C. After cooling to room temperature, 3-(4-bromo-2-trifluoromethyl-phenylsulfanyl)-propionamide (8.0 g, 24.4 mmol), potassium carbonate (8.0 g, 57.9 mmol), dimethylformamide (20 mL), and water (16 mL) were added. The mixture was degassed, stirred for 30 min at room temperature and further [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (400 mg, 547·mol) was added. The resulting brown reaction mixture was stirred for 20 h at 60° C. After cooling to room temperature, it was poured onto water (150 mL) and extracted with ethyl acetate (1×80 mL, 2×40 mL). The combined organic extracts were washed with brine/water (1:1 v/v, mL) and brine (20 mL), methanol (16 mL) was added and the mixture was dried over sodium sulfate. Silica gel (16 g) was added, the slurry was filtered and washed with ethyl acetate/methanol (9:1 v/v, 40 mL). The combined filtrates were concentrated in vacuo. The residue was treated with toluene/n-heptane (1:1 v/v, 24 mL) and the resulting suspension was stirred for 30 min at room temperature. After filtration, the precipitate was washed with toluene/n-heptane (4:1 v/v, 10 mL) and n-heptane (10 mL) and dried in vacuo to afford the title compound as brown crystals (5.7 g, 71%). MS (EI): m/z=341.1 [M+H]+. 1H NMR (d6-DMSO, 400 MHz): δ 2.48 (t, J=7.2 Hz, 2H), 2.54 (s, 3H), 3.32 (t, J=7.2 Hz, 2H), 6.95 (bs, 1H), 7.41 (bs, 1H), 7.58 (dd, J=1.6 Hz, 5.4 Hz, 1H), 7.68 (s, 1H), 7.77 (d, J=9.1 Hz, 1H), 8.02-8.08 (m, 2H), 8.52 (d, J=5.1 Hz, 1H).

後処理

  1. additionwere added at room temperature
  2. customThe solution was degassed
  3. temperatureAfter cooling to room temperature
  4. customThe mixture was degassed
  5. stirringstirred for 30 min at room temperature
  6. additionfurther [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (400 mg, 547·mol) was added
  7. stirringThe resulting brown reaction mixture was stirred for 20 h at 60° C
  8. temperatureAfter cooling to room temperature
  9. additionit was poured onto water (150 mL)
  10. extractionextracted with ethyl acetate (1×80 mL, 2×40 mL)
  11. washThe combined organic extracts were washed with brine/water (1:1 v/v, mL) and brine (20 mL), methanol (16 mL)
  12. additionwas added
  13. dry with materialthe mixture was dried over sodium sulfate
  14. additionSilica gel (16 g) was added
  15. filtrationthe slurry was filtered
  16. washwashed with ethyl acetate/methanol (9:1 v/v, 40 mL)
  17. concentrationThe combined filtrates were concentrated in vacuo
  18. additionThe residue was treated with toluene/n-heptane (1:1 v/v, 24 mL)
  19. stirringthe resulting suspension was stirred for 30 min at room temperature
  20. filtrationAfter filtration
  21. washthe precipitate was washed with toluene/n-heptane (4:1 v/v, 10 mL) and n-heptane (10 mL)
  22. customdried in vacuo

出典と根拠

ORDレコード
ord-56cb95a71a56409abae3c2b7c81a52b4
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08796471B2

反応ノート

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