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Iodide Ion → HCID 69507850、化合物

HRID 1375652
ノート
印刷プレビュー

反応式

HRID 1375652 の反応式
C([SnH2][C:6]1[O:10][N:9]=[C:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:7]=1)(C)(C)C.I[C:17]1[CH:18]=[C:19](/[CH:23]=[CH:24]/[CH2:25][OH:26])[CH:20]=[CH:21][CH:22]=1.O1C=CC=C1P(C1OC=CC=1)C1OC=CC=1.[I-].[F-].[K+]>CN(C=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[OH:26][CH2:25]/[CH:24]=[CH:23]/[C:19]1[CH:18]=[C:17]([C:6]2[O:10][N:9]=[C:8]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:7]=2)[CH:22]=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 30165Iodide IonHCID 521585Tris(furan-2-yl)phosphaneHCID 522689Potassium FluorideHCID 58787323HCID 58787323、化合物HCID 87867900HCID 87867900、化合物

生成物 1

HCID 69507850HCID 69507850、化合物収率 77.8%

試薬・触媒・溶媒 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 6228Dimethylformamide溶媒

実験手順

The tributyltin reagent from Example 1C (665 μL, 1.83 mmol) was added under nitrogen atmosphere to a mixture of alcohol from Example 1B (433 mg, 1.66 mmol), tris(dibenzylideneacetone)-dipalladium(0) (76 mg, 0.083 mmol), tri-2-furylphosphine (39 mg, 0.166 mmol), and cupper(I) iodide (32 mg, 0.166 mmol) in DMF (7 mL). The reaction mixture was stirred at ambient temperature for 30 minutes. Aqueous potassium fluoride was added to the mixture and the resulting suspension was filtered through celite and washed with ethyl acetate. The filtrate was taken up in ethyl acetate and water. The organic phase was washed with brine (×3), dried (MgSO4), filtered and concentrated under reduced pressure and purified by flash chromatography on silica gel with hexane/ethyl acetate (1:1) to provide the titled compound (353 mg). MS (ESI(+)) m/e 291 (M+18)+; 1H NMR (500 MHz, DMSO-d6) δ 8.05(t, J=1.7 Hz, 1H), 7.80 (dt, J1=1.7 Hz, J2=7.5 Hz, 1H), 7.60 (dt, J1=1.7 Hz, J2=7.5 Hz, 1H), 7.57 (s, 1H), 7.51(t, J=7.5 Hz, 1H), 6.63–6.59 (m, 2H), 4.94 (t, J=5.4 Hz, 1H), 4.41 (q, J=7.1 Hz, 2H), 4.19–4.14(m, 2H), 1.35 (t, J=7.1 Hz, 3H).

後処理

  1. filtrationthe resulting suspension was filtered through celite
  2. washwashed with ethyl acetate
  3. washThe organic phase was washed with brine (×3)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. custompurified by flash chromatography on silica gel with hexane/ethyl acetate (1:1)

出典と根拠

ORDレコード
ord-2ad8b7def229499bba3e7af2d350ff14
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07169797B2

反応ノート

読み込み中…

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