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Toluene → HCID 18361476, 화합물

HRID 1166537
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HRID 1166537 반응식
[ClH:1].Br[C:3]1[CH:25]=[CH:24][C:6]([CH2:7][O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[CH2:15][CH:14]([CH2:19][CH2:20][N:21]([CH3:23])[CH3:22])[CH2:13][CH2:12]3)=[CH:5][CH:4]=1.[C:26]1([CH3:32])[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.C(=O)([O-])[O-].[Na+].[Na+].B(O)(O)O.CC1C=CC=CC=1>O.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(O)C>[ClH:1].[CH3:22][N:21]([CH2:20][CH2:19][CH:14]1[CH2:13][CH2:12][C:11]2[C:16](=[CH:17][CH:18]=[C:9]([O:8][CH2:7][C:6]3[CH:24]=[CH:25][C:3]([C:29]4[CH:30]=[CH:31][C:26]([CH3:32])=[CH:27][CH:28]=4)=[CH:4][CH:5]=3)[CH:10]=2)[CH2:15]1)[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 1140TolueneHCID 10340Sodium CarbonateHCID 18361483(+)-6-(4-Bromobenzyl)oxy-2-[2-(N,N-dimethylamino)ethyl]tetralin hydrochlorideHCID 187641984-Methylbenzeneboric acid

생성물 1

HCID 18361476HCID 18361476, 화합물

시약·촉매·용매 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
촉매
HCID 702Ethanol용매
HCID 962Water용매

실험 절차

A mixture of (+)-6-(4-bromobenzyl)oxy-2-[2-(N,N-dimethylamino) ethyl]tetralin hydrochloride (1 g), toluene (20 ml), ethanol (2.5 ml), and 2 M aqueous sodium carbonate (2.5 ml) was stirred at room temperature for 10 min. 4-Methylbenzeneboric acid (416 mg) and tetrakis(triphenylphosphine) palladium (82 mg) were added and the reaction mixture was heated under reflux for 5 hr under argon. After cooling, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried, and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate:hexane=1:40 to 1:4) and converted into its hydrochloride, which was then recrystallized from methanol-diisopropyl ether to obtain the titled compound (660 mg).

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 5 hr under argon
  3. temperatureAfter cooling
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with saturated aqueous sodium chloride
  6. customdried
  7. concentrationconcentrated
  8. customThe residue was purified by alumina column chromatography (eluent: ethyl acetate:hexane=1:40 to 1:4)
  9. customwas then recrystallized from methanol-diisopropyl ether

출처 및 근거

ORD 기록
ord-ba322c785f174b46884e0edc7d15f3db
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06613805B2

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