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Ethanolamine → (E)-3-(5-Bromo-2-methoxy-phenyl)-N-{2-[4-(4-chloro-benzoyl)-piperidin-1-yl]-ethyl}-acrylamide

HRID 434296
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HRID 434296 반응식
N[CH2:2][CH2:3][OH:4].C(O[BH-](O[C:15](=[O:17])[CH3:16])OC(=O)C)(=O)C.[Na+].II.[NH:21]1[CH:25]=[CH:24][N:23]=[CH:22]1.[C:26]1(P(C2C=CC=CC=2)C2C=CC=CC=2)[CH:31]=CC=[CH:28][CH:27]=1.Cl.[Cl:46][C:47]1[CH:52]=[CH:51]C(C(C2CCNCC2)=O)=[CH:49][CH:48]=1.C(N(C(C)C)CC)(C)C.[Br:70][C:71]1[CH:72]=[CH:73][C:74]([O:82][CH3:83])=[C:75](/[CH:77]=C/C(O)=O)[CH:76]=1.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1>CO.ClCCl.CN(C=O)C>[Br:70][C:71]1[CH:72]=[CH:73][C:74]([O:82][CH3:83])=[C:75](/[CH:77]=[CH:2]/[C:3]([NH:21][CH2:25][CH2:24][N:23]2[CH2:28][CH2:27][CH:26]([C:15](=[O:17])[C:16]3[CH:51]=[CH:52][C:47]([Cl:46])=[CH:48][CH:49]=3)[CH2:31][CH2:22]2)=[O:4])[CH:76]=1
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참가 물질

12

반응물 9

HCID 700EthanolamineHCID 795ImidazoleHCID 807IodineHCID 11776TriphenylphosphineHCID 81531Diisopropylethylamine2회HCID 676162trans-5-Bromo-2-methoxycinnamic acidHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate
HCID 27771144-(4-Chlorobenzoyl)piperidine hydrochloride
HCID 5049666Sodium triacetoxyborohydride

생성물 1

HCID 10229092(E)-3-(5-Bromo-2-methoxy-phenyl)-N-{2-[4-(4-chloro-benzoyl)-piperidin-1-yl]-ethyl}-acrylamide

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 21226129Dichloromethane methanol용매

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온도
20 °C

실험 절차

To a suspension of 2-(formyl-3-methoxyphenoxy)ethyl polystyrene (AMEBA) resin (ex Novabiochem) (6.85 g, 3.33 mmol) in a mixture of methanol/dichloromethane (60 ml, 1:1 v/v) is added 2-amino ethanol and sodium triacetoxyborohydride (4.00 g, 18.85 mmol) and the mixture shaken for 16 hours at 20° C., then filtered. The resin is washed with methanol, DMF and dichloromethane, then dried under vacuum. A THF/acetonitrile mixture (50 ml, 1:1 v/v) is added to the dried resin followed by iodine (4.80 g, 18.85 mmol), imidazole (1.28 g, 18.85 mmol) and triphenylphosphine (4.90 g,18.85 mmol). The suspension obtained is shaken for 18 hours at 20° C., then filtered. The resin is washed with THF and dried under vacuum. To the freshly prepared resin (0.50 g, 0.35 mmol) is added a solution of (4-chloro-phenyl)-piperidin-4-yl-methanone hydrochloride (0.18 g, 0.70 mmol) dissolved in DMF (2 ml) and diisopropylethylamine (0.36 g, 2.8 mmol). The mixture is heated at 50° C. for 16 hours and then filtered. The resin is washed with DMF. To the washed resin are added (E)-3-(5-Bromo-2-methoxy-phenyl)-acrylic acid (0.27 g, 1.05 mmol), 2-(1H benzotriazol-1-yl)-1,1,3,3,-tetramethyluronium tetrafluoroborate (0.34 g, 1.05 mmol), diisopropylethylamine (0.29 g, 1.05 mmol) and DMF (4 ml) and the mixture is shaken at 20° C. for 16 hours, then washed with DMF and methanol, after which it is treated with trifluoroacetic acid/dichloromethane (6 ml, 1:1 v/v) at 20° C. for 1 hour to remove the product from the resin. The resulting mixture is filtered and the filtrate evaporated under vacuum to give the product, [MH]+506.7.

후처리

  1. filtrationfiltered
  2. washThe resin is washed with methanol, DMF and dichloromethane
  3. customdried under vacuum
  4. additionA THF/acetonitrile mixture (50 ml, 1:1 v/v) is added to the dried resin
  5. customThe suspension obtained
  6. stirringis shaken for 18 hours at 20° C.
  7. filtrationfiltered
  8. washThe resin is washed with THF
  9. customdried under vacuum
  10. temperatureThe mixture is heated at 50° C. for 16 hours
  11. filtrationfiltered
  12. washThe resin is washed with DMF
  13. stirringthe mixture is shaken at 20° C. for 16 hours
  14. washwashed with DMF and methanol
  15. additionafter which it is treated with trifluoroacetic acid/dichloromethane (6 ml, 1:1 v/v) at 20° C. for 1 hour
  16. customto remove the product from the resin
  17. filtrationThe resulting mixture is filtered
  18. customthe filtrate evaporated under vacuum
  19. customto give the product, [MH]+506.7

출처 및 근거

ORD 기록
ord-8abbccf5430a4c708a5d61e9ba086017
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06670379B2

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