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Butylamine → N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylamine hydrochloride

HRID 1248928
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HRID 1248928 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([Cl:13])[C:5]2[O:9][CH:8]([CH2:10]Br)[CH2:7][C:6]=2[CH:12]=1.[CH2:14]([NH2:18])[CH2:15][CH2:16][CH3:17]>>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([Cl:13])[C:5]2[O:9][CH:8]([CH2:10][NH:18][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:7][C:6]=2[CH:12]=1
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참가 물질

3

반응물 2

HCID 8007ButylamineHCID 135633145,7-Dichloro-2,3-dihydrobenzofuran-2-ylmethyl bromide

생성물 1

HCID 13563316N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylamine hydrochloride

실험 절차

33 g (0.118 mole) of 5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl bromide and 200 ml of n-butylamine were stirred for 12 hours at 60° C. The mixture was evaporated down under reduced pressure, 100 ml of a 20% strength aqueous sodium hydroxide solution were added to the residue, and the mixture was then extracted by shaking with 300 ml of methylene chloride. The organic phase was washed with three times 70 ml of water, dried and evaporated down, the residue was dissolved in 300 ml of dry diethyl ether, the solution was gassed with dry hydrogen chloride at from 0° to +3° C., and the colorless crystalline precipitate was filtered off under suction, washed with dry diethyl ether and dried. 27 g of N-(5,7-dichloro-2,3-dihydrobenzofuran-2-ylmethyl)-N-butylamine hydrochloride of melting point 202°-205° C. were obtained.

후처리

  1. customThe mixture was evaporated down under reduced pressure, 100 ml of a 20% strength aqueous sodium hydroxide solution
  2. additionwere added to the residue
  3. extractionthe mixture was then extracted
  4. washThe organic phase was washed with three times 70 ml of water
  5. customdried
  6. customevaporated down
  7. dissolutionthe residue was dissolved in 300 ml of dry diethyl ether
  8. customwas gassed with dry hydrogen chloride at from 0° to +3° C.
  9. filtrationthe colorless crystalline precipitate was filtered off under suction
  10. washwashed with dry diethyl ether
  11. customdried

출처 및 근거

ORD 기록
ord-2568e150868a46d8bc01d9dddfe00db2
출처 데이터셋
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04628058

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