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Hydrochloric Acid → [Allyl-(5,6-dichloro-pyridin-3-yl)-amino]-acetaldehyde

HRID 1782418
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HRID 1782418 반응식
[CH2:1]([N:4]([C:11]1[CH:12]=[N:13][C:14]([Cl:18])=[C:15]([Cl:17])[CH:16]=1)[CH2:5][CH:6](OC)[O:7]C)[CH:2]=[CH2:3].Cl.ClCCl>O1CCCC1.O>[CH2:1]([N:4]([CH2:5][CH:6]=[O:7])[C:11]1[CH:12]=[N:13][C:14]([Cl:18])=[C:15]([Cl:17])[CH:16]=1)[CH:2]=[CH2:3]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 57448418Allyl-(5,6-dichloro-pyridin-3-yl)-(2,2-dimethoxy-ethyl)amine

생성물 1

HCID 57448419[Allyl-(5,6-dichloro-pyridin-3-yl)-amino]-acetaldehyde

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran
용매

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온도
15 °C

실험 절차

A solution of allyl-(5,6-dichloro-pyridin-3-yl)-(2,2-dimethoxy-ethyl)-amine (57.2 g) in tetrahydrofuran (443 g) was cooled to 10° C. A solution of concentrated hydrochloric acid (136 g) in water (114 g) was slowly added, maintaining the temperature below 20° C. The reaction was then stirred at 15° C. for about 4 hours. Then dichloromethane (570 g) and water (430 g) were added and the layers separated. The organic layer was washed with 5% aqueous sodium bicarbonate (453 g), and then washed twice with water (430 g). The organic layer was concentrated and the residue dissolved in dichloromethane (580 g).

후처리

  1. temperaturemaintaining the temperature below 20° C
  2. customthe layers separated
  3. washThe organic layer was washed with 5% aqueous sodium bicarbonate (453 g)
  4. washwashed twice with water (430 g)
  5. concentrationThe organic layer was concentrated
  6. dissolutionthe residue dissolved in dichloromethane (580 g)

출처 및 근거

ORD 기록
ord-d0b64ee6af274a6b84d05e1bcbe933c0
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07498444B2

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