反応式
[Cl-].[Cl:2][C:3]1[CH:28]=[C:27]([O:29][CH3:30])[C:26]([CH3:31])=[C:25]([Cl:32])[C:4]=1[CH2:5][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.ClC1C(C)=C(OC)C=C(Cl)C=1CCl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:65]([O:67][C:68](=[O:79])[CH:69]=[C:70]([CH3:78])[CH:71]=[CH:72][CH:73]=[C:74]([CH:76]=O)[CH3:75])[CH3:66].C1OC1CC>C1(C)C=CC=CC=1.CCCCCC>[CH2:65]([O:67][C:68](=[O:79])[CH:69]=[C:70]([CH3:78])[CH:71]=[CH:72][CH:73]=[C:74]([CH3:76])[CH:75]=[CH:5][C:4]1[C:25]([Cl:32])=[C:26]([CH3:31])[C:27]([O:29][CH3:30])=[CH:28][C:3]=1[Cl:2])[CH3:66]参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
100 g. of 2,6-dichloro-4-methoxy-5-methyl-benzyl-triphenylphosphonium chloride, prepared from 52 g. of 2,6-dichloro-4-methoxy-3-methyl-benzyl chloride and 57 g. of triphenylphosphine, are treated with 42 g. of 7-formyl-3-methyl-octa-2,4,6-trien-1-oic acid ethyl ester. After the addition of 120 ml. of 1,2-butylene oxide, the resulting mixture is heated to 80°-85° C. for 4 hours while stirring. The mixture is diluted with toluene/hexane (1:1 parts by volume) and exhaustively extracted with methanol/water (60:40 parts by volume). The resulting solution is evaporated under reduced pressure. The oily residue is purified by adsorption on silica gel using toluene for the elution. 9-(2,6-dichloro-4-methoxy-5-methyl-phenyl)-3,7-dimethyl-nona-2,4,6,8-tetraen-1-oic acid ethyl ester is obtained from the eluate and melts at 100°-101° C. after recrystallization from benzene/hexane (50:50 parts by volume).
後処理
- additionAfter the addition of 120 ml
- extractionexhaustively extracted with methanol/water (60:40 parts by volume)
- customThe resulting solution is evaporated under reduced pressure
- customThe oily residue is purified by adsorption on silica gel
- washfor the elution
出典と根拠
- ORDレコード
- ord-e3a9f53bc67c459d91366ca557797bf1
- 出典データセット
- uspto-grants-1981_05
- 特許番号
- US04267382
関連ノート
読み込み中…