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 69546259、化合物

HRID 1744680
ノート
印刷プレビュー

反応式

HRID 1744680 の反応式
FC(F)(F)S(O[C:7]1[CH2:12][N:11]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:10][CH2:9][C:8]=1[C:20](OCC)=O)(=O)=O.[Cl:27][C:28]1[CH:33]=[CH:32]C(B(O)O)=[CH:30][CH:29]=1.[C:37](=[O:40])([O-])[O-:38].[Na+].[Na+].[C:43]1(C)C=CC=C[CH:44]=1.C(O)C>C(OCC)(=O)C.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]>[Cl:27][C:28]1[CH:29]=[CH:30][C:20]([C:8]2[CH2:9][CH2:10][N:11]([C:13]([O:15][C:16]([CH3:17])([CH3:18])[CH3:19])=[O:14])[CH2:12][C:7]=2[C:37]([O:38][CH2:43][CH3:44])=[O:40])=[CH:32][CH:33]=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

7

反応物 4

HCID 10340Sodium CarbonateHCID 742994-Chlorophenylboronic acidHCID 21863594Toluene ethanolHCID 22228415455954-80-0

生成物 1

HCID 69546259HCID 69546259、化合物

試薬・触媒・溶媒 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A vigorously stirred suspension of the product of step C (1.00 g, 2.48 mmol), 4-chlorophenylboronic acid (0.427 g, 2.73 mmol) and [1,1′-bis(diphenylphosphino)-ferrocene)dichloropalladium(II) (0.102 g, 0.124 mmol) in toluene/ethanol (3:2; 24.0 mL) was degassed via three vacuum/nitrogen ingress cycles and then heated to approximately 80° C. Aqueous 2 M sodium carbonate (3.10 mL, 6.20 mmol) was added dropwise via syringe and the resulting mixture maintained at reflux overnight. After cooling to ambient temperature, the reaction mixture was diluted with ethyl acetate and filtered through celite®. The filtrate was poured into water and extracted three times with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. Purification of the residue by medium pressure liquid chromatography on silica gel (gradient elution; 0–15% ethyl acetate/hexanes as eluent) furnished the title compound as a colorless oil (0.828 g).

後処理

  1. customwas degassed via three vacuum/nitrogen ingress cycles
  2. temperaturethe resulting mixture maintained
  3. temperatureat reflux overnight
  4. temperatureAfter cooling to ambient temperature
  5. filtrationfiltered through celite®
  6. additionThe filtrate was poured into water
  7. extractionextracted three times with ethyl acetate
  8. washThe combined organic extracts were washed with brine
  9. dry with materialdried (MgSO4)
  10. concentrationconcentrated in vacuo
  11. customPurification of the residue by medium pressure liquid chromatography on silica gel (gradient elution; 0–15% ethyl acetate/hexanes as eluent)

出典と根拠

ORDレコード
ord-c528eac3e5104205a8f4c2533514739f
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07015235B2

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