Tetrahydrofuran → HCID 86682689, 화합물

HRID 449784

반응식

HRID 449784 반응식
[O:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:6]([C:8]1[CH:14]=[CH:13][C:11]([OH:12])=[CH:10][C:9]=1[OH:15])[CH3:7].[H-].[Na+].[P:18](Cl)([O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:19]>O>[CH2:5]([O:1][P:18]([O:12][C:11]1[CH:13]=[CH:14][C:8]([CH2:6][CH3:7])=[C:9]([O:15][P:18]([O:28][CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])[CH:10]=1)([O:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:19])[C:4]1[CH:29]=[CH:30][CH:31]=[CH:2][CH:3]=1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 179274-EthylresorcinolHCID 24758Sodium hydrideHCID 4641201(Chloro(phenylmethoxy)phosphoryl)oxymethylbenzene

생성물 1

HCID 86682689HCID 86682689, 화합물수율 84%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

To a tetrahydrofuran solution (10 ml) of 4-ethylresorcinol (423 mg), sodium hydride (60% dispersion in liquid paraffin) (269 mg) was added and stirred at 0° C. for 30 minutes. Then, dibenzyl chlorophosphate (10 w/v % solution in benzene) (20 ml) was added dropwise. After stirring at room temperature for 3 hours, water (10 ml) was added to the reaction mixture, and the extraction was carried out with ethyl acetate (30 ml). Then, the extract was washed with saturated brine (10 ml), dried with anhydrous sodium sulfate and then concentrated. The residue (2.16 g) was subjected to silica gel chromatography (silica gel 60 g, chloroform to chloroform:methanol=50:1), to give 1,3-bis(dibenzylphosphonooxy)-4-ethylbenzene (1.65 g, yield: 84%) as a yellow liquid.

후처리

  1. stirringAfter stirring at room temperature for 3 hours
  2. extractionthe extraction
  3. washThen, the extract was washed with saturated brine (10 ml)
  4. dry with materialdried with anhydrous sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3b038dd0f79844eb9315b9354b832b37
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486919B2

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