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Potassium bisulfate → HCID 10526643, 화합물

HRID 1707817
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HRID 1707817 반응식
[CH3:1][Mg]Br.[F:4][C:5]1[CH:10]=[CH:9][C:8]([C@H:11]([C:21]2[C:26]([O:27][CH3:28])=[C:25]([CH3:29])[C:24]([CH3:30])=[C:23]([CH:31]=[O:32])[C:22]=2[CH3:33])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([O:19][CH3:20])=[O:18])=[CH:7][CH:6]=1.S([O-])(O)(=O)=O.[K+]>O1CCCC1>[F:4][C:5]1[CH:6]=[CH:7][C:8]([C@H:11]([C:21]2[C:26]([O:27][CH3:28])=[C:25]([CH3:29])[C:24]([CH3:30])=[C:23]([CH:31]([OH:32])[CH3:1])[C:22]=2[CH3:33])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([O:19][CH3:20])=[O:18])=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516920Potassium bisulfateHCID 10787945methyl (R)-7-(4-fluorophenyl)-7-(3-formyl-6-methoxy-2,4,5-trimethylphenyl)heptanoateHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 10526643HCID 10526643, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To a solution of methylmagnesium bromide in tetrahydrofuran (1 M, 54.3 ml) was added anhydrous tetrahydrofuran (90 ml). To the solution was added dropwise a solution of methyl (R)-7-(4-fluorophenyl)-7-(3-formyl-6-methoxy-2,4,5-trimethylphenyl)heptanoate (4.5 g, 10.9 mmol) in tetrahydrofuran (20 ml) at -78° C., followed by stirring for 30 minutes at the same temperature. To the reaction mixture, an aqueous solution of potassium hydrogensulfate, followed by subjected to extraction with ethyl acetate. The organic layer was washed with water, an aqueous solution of sodium hydrogencarbonate and water, in the order mentioned, and dried over magnesiumsulfate. The organic layer was distilled off under reduced pressure, and the residue was subjected to a silica gel column chromatography to give methyl (R)-7-(4-fluorophenyl)-7-[3-(1-hydroxyethyl)-6-methoxy-2,4,5-trimethylphenyl]heptanoate (4.4 g). Physico-chemical properties and spectral data of this compound are shown in [Table 5].

후처리

  1. extractionby subjected to extraction with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesiumsulfate
  4. distillationThe organic layer was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-004ad427518640bcab699488cfe9e807
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05354913

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