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Hydrochloric Acid → HCID 86759326, 화합물

HRID 2119281
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HRID 2119281 반응식
[Mg].[CH2:2]([O:9][C:10]1[CH:15]=[CH:14][C:13](Br)=[CH:12][CH:11]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH2:17]([CH:21]1[CH2:26][CH2:25][CH:24](C2CCC(=O)CC2)[CH2:23][CH2:22]1)[CH2:18][CH2:19][CH3:20].Cl>C1COCC1>[CH2:17]([CH:21]1[CH2:26][CH2:25][CH:24]([C:12]2[C:11]([C:10]3([OH:9])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]3)=[C:10]([O:9][CH2:2][C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[CH:15]=[CH:14][CH:13]=2)[CH2:23][CH2:22]1)[CH2:18][CH2:19][CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1388351-Bromo-4-phenylmethoxybenzeneHCID 5462224MagnesiumHCID 234403784'-Butyl(1,1'-bi(cyclohexane))-4-one

생성물 1

HCID 86759326HCID 86759326, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To the Grignard reagent which was prepared from 2.31 g (95.1 mmol) of dried magnesium and 25.0 g (95.0 mmol) of 4-benzyloxy-bromobenzene in 300 ml of THF, was added dropwise 100 ml of solution of 21.0 g (88.8 mmol) of 4-(4-n-butylcyclohexyl)-cyclohexanone in THF at room temperature, and the mixture was stirred at the same temperature for 12 hours. The reaction solution was added to 500 ml of 0.5N hydrochloric acid, the product thus formed was extracted with ether, the extract was washed with saturated aqueous sodium bicarbonate solution and water in this turn, and then the solvent was distilled off. After the residue was purified by column chromatography on silica gel (eluent: toluene), the solvent was distilled off, and the residue was recrystallized from toluene to give 11.8 g (28.1 mmol) of 4-(4-(4-n-butyl-cyclohexyl(-1-hydroxycyclohexyl)-1-benzyloxybenzene. Yield of this compound based on 4-(4-n-butylcyclohexyl)cyclohexanone was 31.6%.

후처리

  1. customthe product thus formed
  2. extractionwas extracted with ether
  3. washthe extract was washed with saturated aqueous sodium bicarbonate solution and water in this turn
  4. distillationthe solvent was distilled off
  5. customAfter the residue was purified by column chromatography on silica gel (eluent: toluene)
  6. distillationthe solvent was distilled off
  7. customthe residue was recrystallized from toluene

출처 및 근거

ORD 기록
ord-a37f625a563c4112b9460929df0dc085
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06685995B1

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