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Benzo(B)Thiophene → (2-Benzo[b]thiophen-2-yl-ethyl)-dimethylamine

HRID 746599
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HRID 746599 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH:3]=[CH:2]1.[Li]CCCC.Br.[CH3:16][N:17]([CH3:21])[CH2:18][CH2:19]Br>C1COCC1>[S:1]1[C:2]([CH2:19][CH2:18][N:17]([CH3:21])[CH3:16])=[CH:3][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]1=2
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참가 물질

5

반응물 3

HCID 7221Benzo(B)ThiopheneHCID 457913472-Bromoethyldimethylammonium bromideHCID 178418339Butyllithium

생성물 1

HCID 58591561(2-Benzo[b]thiophen-2-yl-ethyl)-dimethylamine수율 65%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

To a cooled (−78° C.) solution of benzothiophene (74.5 mmol) in anhydrous THF (100 mL) was added slowly n-BuLi (82 mmol, 1.6 M in hexanes). The mixture was stirred at −78° C. for 1 hr. β-Dimethylaminoethyl bromide hydrobromide (41 mmol) was added at −78° C. and the temperature was allowed to reach 0° C. over 5 hours. The mixture was quenched in sat. NH4Cl, the pH of the aqueous layer was adjusted to 7-8 with sat. NaHCO3, and the mixture was extracted with EtOAc (4×). The combined organic layers were concentrated and extracted with 1N HCl (3×). The combined HCl layers were made basic with sat. NaHCO3, extracted with EtOAc (4×), and the combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated in vacuo to afford Compound 1a (2-Benzo[b]thiophen-2-yl-ethyl)-dimethyl-amine (4.96 g, 65%) as a tan solid; MS (MH+)=206.

후처리

  1. waitto reach 0° C. over 5 hours
  2. customThe mixture was quenched in sat. NH4Cl
  3. extractionthe mixture was extracted with EtOAc (4×)
  4. concentrationThe combined organic layers were concentrated
  5. extractionextracted with 1N HCl (3×)
  6. extractionextracted with EtOAc (4×)
  7. washthe combined organic layers were washed with brine
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6d3d4bee1ea2456198465e9722e4f461
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07393865B2

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