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Cyclopropanecarboxaldehyde → N-(Cyclopropyhnethyl)-N-{2-[4-(3,4-difluorophenoxy)-1-piperidinyl]ethyl}amine

HRID 968761
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HRID 968761 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][C:17]=1[F:18])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][NH2:14])[CH2:8][CH2:7]1.[CH:19]1([CH:22]=O)[CH2:21][CH2:20]1>CO>[CH:19]1([CH2:22][NH:14][CH2:13][CH2:12][N:9]2[CH2:8][CH2:7][CH:6]([O:5][C:4]3[CH:15]=[CH:16][C:17]([F:18])=[C:2]([F:1])[CH:3]=3)[CH2:11][CH2:10]2)[CH2:21][CH2:20]1
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참가 물질

4

반응물 2

HCID 123114CyclopropanecarboxaldehydeHCID 693106352-[4-(3,4-Difluorophenoxy)-1-piperidinyl]ethylamine

생성물 1

HCID 70015962N-(Cyclopropyhnethyl)-N-{2-[4-(3,4-difluorophenoxy)-1-piperidinyl]ethyl}amine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The product of Step d (0.4 g) dissolved in MeOH (6 ml) was added to cyclopropanecarbaldehyde (0.116 ml) and the resulting mixture was stirred for 4 hours. The solvent was evaporated, the residue re-dissolved in methanol (6 ml) and NaBH4 (0.095 g) added and the mixture left for 30 minutes. Aqueous sodium hydroxide (1N) was added and the aqueous extracted with diethyl ether. The organic extracts were dried with Na2SO4, filtered and concentrated to give the sub-title product as an oil (0.493 g).

후처리

  1. customThe solvent was evaporated
  2. dissolutionthe residue re-dissolved in methanol (6 ml)
  3. additionNaBH4 (0.095 g) added
  4. waitthe mixture left for 30 minutes
  5. additionAqueous sodium hydroxide (1N) was added
  6. extractionthe aqueous extracted with diethyl ether
  7. dry with materialThe organic extracts were dried with Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-331e1f71b3e442c1bc4d25e8a8cec63a
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07304077B2

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