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Hydrochloric Acid → HCID 178444343, 화합물

HRID 635771
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HRID 635771 반응식
[Mg].[CH2:2]([C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]2[CH:18]=[CH:17][C:16](Br)=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)[CH2:3][CH2:4][CH2:5][CH3:6].[C:20](=[S:22])=[S:21].Cl>C1COCC1>[CH2:2]([C@H:7]1[CH2:12][CH2:11][C@H:10]([C:13]2[CH:18]=[CH:17][C:16]([C:20]([SH:22])=[S:21])=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)[CH2:3][CH2:4][CH2:5][CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6348Carbon DisulfideHCID 5462224MagnesiumHCID 178444243HCID 178444243, 화합물

생성물 1

HCID 178444343HCID 178444343, 화합물수율 51.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension prepared by suspending 0.95 g (39 mmol) of magnesium in 200 ml of THF was added dropwise a solution prepared by dissolving 9.28 g (30 mmol) of 4-(trans-4-n-pentylcyclohexyl)bromobenzene in 80 ml of THF, at room temperature while being stirred in 1 hour, and then heated to reflux for 2 hours to prepare a Grignard reagent. To this solution was added dropwise 5.7 g (75 mmol) of carbon disulfide at room temperature in 30 min and stirred as it was overnight. To this reaction solution was added 150 ml of 1M hydrochloric acid to terminate the reaction and extracted with 350 ml of toluene. The organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under a reduced pressure, and the residue was recrystallized from heptane to obtain 4.74 g of 4-(trans-4-n-pentylcyclohexyl)phenyldithiocarboxylic acid (yield 51.5%).

후처리

  1. customTo a suspension prepared
  2. additionwas added dropwise a solution
  3. customprepared
  4. temperatureheated
  5. temperatureto reflux for 2 hours
  6. stirringstirred as it
  7. waitwas overnight
  8. customto terminate
  9. customthe reaction
  10. extractionextracted with 350 ml of toluene
  11. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  12. distillationthe solvent was distilled off under a reduced pressure
  13. customthe residue was recrystallized from heptane

출처 및 근거

ORD 기록
ord-d9a6145e47514282a3f80963d8dd5e91
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06190576B1

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