p-Toluenesulfonic acid → 1-(4'-Pentyl-2-fluorobiphenyl-4-yl)-2-(5-heptyl-1,3-dioxan-2-yl)-ethane

HRID 246871

反応式

[CH2:1]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH:20]=[O:21])=[CH:14][C:13]=2[F:22])=[CH:8][CH:7]=1)[CH2:2][CH2:3][CH2:4][CH3:5].C1OC1.[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.[CH2:37]([CH:44]([CH2:47]O)[CH2:45][OH:46])[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.O>[CH2:1]([C:6]1[CH:7]=[CH:8][C:9]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH:20]3[O:46][CH2:45][CH:44]([CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[CH2:47][O:21]3)=[CH:14][C:13]=2[F:22])=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH3:5]

参加物

実験手順

6 g of 3-(4'-pentyl-2-fluorobiphenyl-4-yl)-propionaldehyde (obtainable by reaction of 4-(2-fluoro-4'-pentylbiphenylyl)-magnesium bromide with ethylene oxide and subsequent oxidation of the resulting alcohol with pyridinium chlorochromate) and 3.5 g of 2-heptylpropane-1,3-diol are heated with a spatula tip of p-toluenesulfonic acid in 100 ml of toluene, using a water separator, until no further water is foamed. After cooling, the mixture is washed with bicarbonate solution and water until neutral and dried over sodium sulfate and the toluene is distilled off. After customary working-up, 1-(4'-pentyl-2-fluorobiphenyl-4-yl)-2-(5-heptyl-1,3-dioxan-2-yl)-ethane is obtained.

後処理

temperatureAfter cooling
washthe mixture is washed with bicarbonate solution and water until neutral and
dry with materialdried over sodium sulfate
distillationthe toluene is distilled off

出典と根拠

ORDレコード: ord-4b3486c85a834ce6bb8d008df64f872d
出典データセット: uspto-grants-1987_11
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04704227

反応式

参加物

反応物 5

生成物 1

試薬・触媒・溶媒 2

実験手順

後処理

出典と根拠

関連ノート