反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1CCN(C(N=NC(N2CCCCC2)=O)=O)CC1.[N:38]1[CH:43]=[CH:42][CH:41]=[C:40]([C:44]2[CH:49]=[CH:48][C:47]([C:50]([C:54]3[CH:59]=[CH:58][C:57]([C:60]4[CH:61]=[N:62][CH:63]=[CH:64][CH:65]=4)=[CH:56][CH:55]=3)=[CH:51][CH2:52]O)=[CH:46][CH:45]=2)[CH:39]=1.[CH2:66]([O:68][C:69](=[O:83])[CH2:70][O:71][C:72]1[CH:77]=[CH:76][C:75]([SH:78])=[CH:74][C:73]=1[C:79]([F:82])([F:81])[F:80])[CH3:67]>C1COCC1>[CH2:66]([O:68][C:69](=[O:83])[CH2:70][O:71][C:72]1[CH:77]=[CH:76][C:75]([S:78][CH2:52][CH:51]=[C:50]([C:54]2[CH:59]=[CH:58][C:57]([C:60]3[CH:61]=[N:62][CH:63]=[CH:64][CH:65]=3)=[CH:56][CH:55]=2)[C:47]2[CH:46]=[CH:45][C:44]([C:40]3[CH:39]=[N:38][CH:43]=[CH:42][CH:41]=3)=[CH:49][CH:48]=2)=[CH:74][C:73]=1[C:79]([F:80])([F:81])[F:82])[CH3:67]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
Triphenylphosphine (138 mg, 0.68 mmol) and ADDP (173 mg, 0.68 mmol) were added to a solution of 3,3-bis-(4-pyridin-3-yl-phenyl)-prop-2-en-1-ol (100 mg, 0.27 mmol) in THF (5 ml) at 0° C. The reaction mixture was stirred for 5 min under nitrogen atmosphere. (4-Mercapto-2-trifluoromethyl-phenoxy)-acetic acid ethyl ester (prepared analogous to procedure in BioOrg. Med. Chem. Lett. 2003, 13, 1517) (92 mg, 0.32 mmol) was slowly added to the reaction mixture and the reaction was stirred for further 2 h at 0° C. The reaction mixture was evaporated and the residue was triturated with ether (2×15 ml). The filtered ether phases were evaporated and purified by column chromatography (eluent: ethyl acetate) to give {4-[3,3-bis-(4-pyridin-3-yl-phenyl)-allylsulfanyl]-2-trifluoromethyl-phenoxy}-acetic acid ethyl ester in 100 mg (60%) yield.
後処理
- stirringthe reaction was stirred for further 2 h at 0° C
- customThe reaction mixture was evaporated
- customthe residue was triturated with ether (2×15 ml)
- customThe filtered ether phases were evaporated
- custompurified by column chromatography (eluent: ethyl acetate)
出典と根拠
- ORDレコード
- ord-c5ebe0b0aed846cc89d4466e7663f9a1
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091245B2
関連ノート
読み込み中…