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2-Bromo-m-xylene → (1-(2,6-Dimethylphenyl)pyrrolidin-3-yl)methanol

HRID 1041887
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HRID 1041887 반응식
Br[C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH3:9].Cl.[NH:11]1[CH2:15][CH2:14][CH:13]([CH2:16][OH:17])[CH2:12]1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.C[Si](C)(C)[N-][Si](C)(C)C.[Li+].O.C(=O)(O)[O-].[Na+]>O1CCCC1.[Pd].C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(OCC)(=O)C>[CH3:9][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([CH3:8])[C:2]=1[N:11]1[CH2:15][CH2:14][CH:13]([CH2:16][OH:17])[CH2:12]1
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참가 물질

9

반응물 5

HCID 684712-Bromo-m-xyleneHCID 2733832Lithium hexamethyldisilazaneHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 23080030(Pyrrolidin-3-yl)methanol hydrochlorideHCID 86585896Sodium bicarbonate water

생성물 1

HCID 24275467(1-(2,6-Dimethylphenyl)pyrrolidin-3-yl)methanol
수율 27.8%

시약·촉매·용매 3

HCID 1542701,5-Diphenylpenta-1,4-dien-3-one;palladium촉매HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 2-bromo-1,3-dimethylbenzene (500 mg), pyrrolidine-3-yl methanol hydrochloride (409 mg), bis(dibenzylideneacetone) palladium (155 mg), and 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (SPhos; 222 mg) in tetrahydrofuran (5 mL), molecular sieves 4A (powder; 410 mg) were added. To the mixed solution, a solution (8.9 mL) of 1.0 M lithium hexamethyldisilazide in tetrahydrofuran was added, and the resultant reaction mixture was heated and refluxed for 2.5 hours. To the reaction solution, saturated sodium bicarbonate water and ethyl acetate were added, and the resultant reaction mixture was extracted with ethyl acetate. The organic phase was washed with a saturated saline and was dried over anhydrous sodium sulfate. From the organic phase, the solvent was distilled off under reduced pressure, followed by purifying the resultant residue by silica gel column chromatography (eluate; n-hexane:ethyl acetate=100:0 to 75:25), and from the resultant, the solvent was distilled off under reduced pressure to obtain the subject compound (154 mg) as a yellow oily substance.

후처리

  1. customthe resultant reaction mixture
  2. temperaturewas heated
  3. temperaturerefluxed for 2.5 hours
  4. customthe resultant reaction mixture
  5. extractionwas extracted with ethyl acetate
  6. washThe organic phase was washed with a saturated saline
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. distillationFrom the organic phase, the solvent was distilled off under reduced pressure
  9. customby purifying the resultant residue by silica gel column chromatography (eluate; n-hexane:ethyl acetate=100:0 to 75:25)
  10. distillationfrom the resultant, the solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-2715480677eb467bbf840d884a863e98
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08557766B2

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