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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
ノート
印刷プレビュー

反応式

HRID 434296 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

12

反応物 9

HCID 700EthanolamineHCID 795ImidazoleHCID 807IodineHCID 11776TriphenylphosphineHCID 81531Diisopropylethylamine2 回HCID 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 21226129Dichloromethane methanol溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8abbccf5430a4c708a5d61e9ba086017
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06670379B2

反応ノート

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