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Cesium carbonate → methyl 3-phenyl-2-{[6-(5-phenyl-1H-pyrrol-2-yl)-2-naphthyl]oxy}propanoate

HRID 456814
ノート
印刷プレビュー

反応式

HRID 456814 の反応式
[C:1]1([C:7]2[NH:11][C:10]([C:12]3[CH:13]=[C:14]4[C:19](=[CH:20][CH:21]=3)[CH:18]=[C:17]([OH:22])[CH:16]=[CH:15]4)=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:23][O:24][C:25](=[O:42])[CH:26](OS(C(F)(F)F)(=O)=O)[CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CC(C)=O>[C:28]1([CH2:27][CH:26]([O:22][C:17]2[CH:16]=[CH:15][C:14]3[C:19](=[CH:20][CH:21]=[C:12]([C:10]4[NH:11][C:7]([C:1]5[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=5)=[CH:8][CH:9]=4)[CH:13]=3)[CH:18]=2)[C:25]([O:24][CH3:23])=[O:42])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 13388932alpha-(Trifluoromethylsulfonyloxy)hydrocinnamic acid methyl esterHCID 184390376-(5-phenyl-1H-pyrrol-2-yl)-2-naphthol

生成物 1

HCID 18439046methyl 3-phenyl-2-{[6-(5-phenyl-1H-pyrrol-2-yl)-2-naphthyl]oxy}propanoate収率 95.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 6-(5-phenyl-1H-pyrrol-2-yl)-2-naphthol (0.300 g, 1.05 mmol), prepared in the previous step, 3-phenyl-2-trifluoromethanesulfonyloxypropionic acid methyl ester (0.492 g, 1.58 mmol) and cesium carbonate (0.685 g, 2.10 mmol) in acetone (50 mL) was stirred under nitrogen at ambient temperature overnight. The acetone was removed under reduced pressure and the residue partitioned between EtOAc and water. The layers were separated and the aqueous layer was extracted two times with EtOAc. The combined extracts were dried (MgSO4), filtered and the solvent removed under reduced pressure. Purification on a Biotage FlashElute™ system with a KP-Sil Flash 40L column (120 g Silica Gel, 60 Å) using 25% to 60% methylene chloride in hexane as the eluent gave methyl 3-phenyl-2-{[6-(5-phenyl-1H-pyrrol-2-yl)-2-naphthyl]oxy}propanoate as a grayish solid (0.447 g, 95%), mp 140–141° C. Elemental Analysis for C30H25NO3 Calc'd: C, 80.51; H, 5.63; N, 3.13. Found: C, 80.26; H, 5.70; N, 2.94.

後処理

  1. customThe acetone was removed under reduced pressure
  2. customthe residue partitioned between EtOAc and water
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted two times with EtOAc
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent removed under reduced pressure
  8. customPurification on a Biotage FlashElute™ system with a KP-Sil Flash 40L column (120 g Silica Gel, 60 Å)

出典と根拠

ORDレコード
ord-28bc9a1f5685414d8b3facbf5ede4050
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07186749B2

反応ノート

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