Tributylvinyltin → HCID 57665494、化合物

反応式

[NH2:1][C:2]1[C:23](I)=[CH:22][C:5]([CH2:6][NH:7][C:8]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:14][CH:13]=2)=[O:9])=[CH:4][C:3]=1[F:25].[CH2:26]([Sn](CCCC)(CCCC)C=C)[CH2:27]CC>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1(C)C=CC=CC=1>[NH2:1][C:2]1[C:23]([CH:26]=[CH2:27])=[CH:22][C:5]([CH2:6][NH:7][C:8]([NH:10][CH2:11][C:12]2[CH:17]=[CH:16][C:15]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:14][CH:13]=2)=[O:9])=[CH:4][C:3]=1[F:25]

参加物

実験手順

To the 50 ml round bottom flask were put 1-(4-amino-3-fluoro-5-iodo-benzyl)-3-(4-t-butyl-benzyl)-urea (0.17 g, 0.37 mmol) and Pd(PPh3)4 (0.05 eq, 21.3 mg). And to this reaction mixture was added 20 ml toluene and tributyl(vinyl)tin (1.1 eq, 0.13 g) by syringe and refluxed for 2 hours. After confirming the completion of the reaction with TLC, the reaction mixture was extracted with ethylacetate, washed with 1M KF solution. And the combined organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (n-hexane/ethyl acetate=2/1).