ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium Carbonate → HCID 178474394、化合物

HRID 1162466
ノート
印刷プレビュー

反応式

HRID 1162466 の反応式
Br[C:2]1[CH:3]=[C:4]([NH:9][S:10]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)(=[O:12])=[O:11])[C:5]([Cl:8])=[N:6][CH:7]=1.B1(B2OC(C)(C)C(C)(C)O2)OC(C)(C)C(C)(C)O1.C([O-])(=O)C.[K+].Br[C:44]1[CH:56]=[CH:55][C:47]2[NH:48][C:49]([NH:51][C:52](=[O:54])[CH3:53])=[N:50][C:46]=2[CH:45]=1.C(=O)([O-])[O-].[Na+].[Na+]>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CN(C=O)C.O1CCOCC1>[Cl:8][C:5]1[N:6]=[CH:7][C:2]([C:56]2[CH:44]=[CH:45][C:46]3[NH:50][C:49]([NH:51][C:52](=[O:54])[CH3:53])=[N:48][C:47]=3[CH:55]=2)=[CH:3][C:4]=1[NH:9][S:10]([C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=1)(=[O:12])=[O:11]
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 10340Sodium CarbonateHCID 517044Potassium AcetateHCID 2733548Bis(pinacolato)diboraneHCID 53363354N-(5-bromo-2-chloropyridin-3-yl)-4-fluorobenzenesulfonamideHCID 178474391HCID 178474391、化合物

生成物 1

HCID 178474394HCID 178474394、化合物収率 15.2%

試薬・触媒・溶媒 3

HCID 178418476HCID 178418476、化合物触媒HCID 6228Dimethylformamide溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

To a 25 mL round-bottomed flask was added N-(5-bromo-2-chloropyridin-3-yl)-4-fluorobenzenesulfonamide (0.150 g, 0.410 mmol) (Step 1, Example 48), bis(pinacolato)diboron (0.156 g, 0.615 mmol, Aldrich, St, Louis, Mo.), potassium acetate (0.161 g, 1.64 mmol) and 1,4-dioxane (4.0 mL). The mixture was carefully evacuated and backfilled with N2. To the solution was added dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium(II)dichloromethane adduct (0.030 g, 0.041 mmol, Strem Chemical, Inc., Newburyport, Mass.). The mixture was carefully evacuated and backfilled with N2 again. The mixture was stirred at 90° C. for 6 h. The reaction mixture was cooled to rt and to it was added DMF (4.0 mL), N-(5-bromo-1H-benzo[d]imidazol-2-yl)acetamide (0.080 g, 0.31 mmol) and aq sodium carbonate (0.79 mL, 1.6 mmol, 2 M). The mixture was carefully evacuated and backfilled with N2. To the mixture was added trans-dichlorobis(triphenylphosphine)palladium(II) (0.022 g, 0.031 mmol, Strem Chemical, Inc., Newburyport, Mass.). Once again the mixture was carefully evacuated and backfilled with N2. The mixture was stirred at 90° C. for 16 h and then, after cooling to rt, was poured into aq. NaCl (100 mL) and extracted with 25% iPrOH/CHCl3 (3×75 mL). The combined extracts were dried (Na2SO4) and concentrated. The material was then taken up in MeOH/CH2Cl2 and concentrated onto silica. Purification by silica gel chromatography (0.5 to 5.0% MeOH (2 M in NH3)/CH2Cl2) afforded the title compound as a white solid (0.0217 g, 15%). MS (ESI, positive ion) m/z: 460 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.18 (s, 3H), 7.37 (br s, 1H), 7.44 (t, J=8.8 Hz, 2H), 7.56 (br s, 1H), 7.70 (br s, 1H), 7.83 (dd, J=8.8, 5.3 Hz, 2H), 7.91 (s, 1H), 8.56 (br s, 1H), 10.44 (br s, 1H), 11.62 (br s, 1H), 12.16 (br s, 1H).

後処理

  1. customThe mixture was carefully evacuated
  2. customThe mixture was carefully evacuated
  3. temperatureThe reaction mixture was cooled to rt and to it
  4. customThe mixture was carefully evacuated
  5. customOnce again the mixture was carefully evacuated
  6. stirringThe mixture was stirred at 90° C. for 16 h
  7. temperatureafter cooling to rt
  8. additionwas poured into aq. NaCl (100 mL)
  9. extractionextracted with 25% iPrOH/CHCl3 (3×75 mL)
  10. dry with materialThe combined extracts were dried (Na2SO4)
  11. concentrationconcentrated
  12. concentrationconcentrated onto silica
  13. customPurification by silica gel chromatography (0.5 to 5.0% MeOH (2 M in NH3)/CH2Cl2)

出典と根拠

ORDレコード
ord-ff1136683c90473796faccef2a65389e
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820665B2

反応ノート

読み込み中…

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