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

HRID 246871

반응식

HRID 246871 반응식
[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]

참가 물질

8

반응물 5

HCID 6101p-Toluenesulfonic acidHCID 6354Ethylene OxideHCID 2255562-Heptylpropane-1,3-diolHCID 201626933-(4'-Pentyl-2-fluorobiphenyl-4-yl)-propionaldehydeHCID 178418287HCID 178418287, 화합물

생성물 1

HCID 201625331-(4'-Pentyl-2-fluorobiphenyl-4-yl)-2-(5-heptyl-1,3-dioxan-2-yl)-ethane

시약·촉매·용매 2

HCID 962Water용매2회HCID 1140Toluene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-4b3486c85a834ce6bb8d008df64f872d
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04704227

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