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Methanol → Benzyl[4-(2-{3-[1-(2-dimethylaminoethyl)piperidin-4-yl]-3-methylureido}pyridin-4-yloxy)-2-fluorophenyl]carbamate

HRID 492876
ノート
印刷プレビュー

反応式

HRID 492876 の反応式
ClC(OC1C=CC=CC=1)=O.[NH2:11][C:12]1[CH:17]=[C:16]([O:18][C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:35])[O:27][CH2:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[C:21]([F:36])[CH:20]=2)[CH:15]=[CH:14][N:13]=1.Cl.Cl.Cl.[CH3:40][N:41]([CH3:52])[CH2:42][CH2:43][N:44]1[CH2:49][CH2:48][CH:47]([NH:50][CH3:51])[CH2:46][CH2:45]1.[OH-:53].[Na+].[CH3:55]O>O1CCCC1.[Cl-].[Na+].O.C(OCC)(=O)C.C(N(CC)CC)C>[CH3:40][N:41]([CH3:52])[CH2:42][CH2:43][N:44]1[CH2:45][CH2:46][CH:47]([N:50]([CH3:55])[C:51](=[O:53])[NH:11][C:12]2[CH:17]=[C:16]([O:18][C:19]3[CH:24]=[CH:23][C:22]([NH:25][C:26](=[O:35])[O:27][CH2:28][C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)=[C:21]([F:36])[CH:20]=3)[CH:15]=[CH:14][N:13]=2)[CH2:48][CH2:49]1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 887MethanolHCID 14798Sodium Hydroxide2 回HCID 15891Phenyl chloroformateHCID 23152980N-[1-(2-dimethylaminoethyl)piperidin-4-yl]-N-methylamine trihydrochlorideHCID 57470855Benzyl[4-(2-aminopyridin-4-yloxy)-2-fluorophenyl]carbamate

生成物 1

HCID 57677742
Benzyl[4-(2-{3-[1-(2-dimethylaminoethyl)piperidin-4-yl]-3-methylureido}pyridin-4-yloxy)-2-fluorophenyl]carbamate
収率 28.4%

試薬・触媒・溶媒 4

HCID 8028Tetrahydrofuran溶媒2 回HCID 8471Triethylamine溶媒2 回HCID 8857Ethyl Acetate溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

After adding triethylamine (0.127 ml) and phenyl chloroformate (0.100 ml) to a solution of benzyl [4-(2-aminopyridin-4-yloxy)-2-fluorophenyl]carbamate (113 mg) in tetrahydrofuran (5.0 ml), the mixture was stirred for 30 minutes at room temperature under a nitrogen atmosphere. The reaction mixture was partitioned between ethyl acetate (50 ml) and brine (30 ml). The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. To this residue was added a suspension (4 ml) produced by adding tetrahydrofuran (6.0 ml) and triethylamine (2.0 ml) to N-[1-(2-dimethylaminoethyl)piperidin-4-yl]-N-methylamine trihydrochloride (673 mg), and the resulting mixture was stirred at room temperature for 27 hours. Ethyl acetate (30 ml) and 1N aqueous sodium hydroxide (10 ml) were added to the reaction mixture, and stirring was carried out for 5 hours at room temperature. Brine was added thereto and the mixture was extracted with ethyl acetate. The aqueous layer was then extracted with ethyl acetate. The organic layers were combined and washed with 1N aqueous sodium hydroxide and brine in that order, and dried over anhydrous sodium sulfate. The dried organic layer was concentrated and the residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate:methanol=20:1 to 10:1). Fractions containing the target compound were concentrated to provide a white solid. Methanol (3 ml) and 5N aqueous sodium hydroxide (1 ml) were added thereto, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was then partitioned between ethyl acetate and brine. The organic layer was washed with brine and then dried over anhydrous sodium sulfate. It was subsequently concentrated. The residue was purified by LC-MS (eluent; acetonitrile-water-trifluoroacetic acid system). Fractions containing the target compound were concentrated, respectively. The residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogencarbonate. The organic layer was dried over anhydrous sodium sulfate. It was then concentrated to provide the title compound (51.3 mg, 28.4%) as a colorless oil.

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate (50 ml) and brine (30 ml)
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. additionTo this residue was added a suspension (4 ml)
  5. customproduced
  6. stirringthe resulting mixture was stirred at room temperature for 27 hours
  7. stirringstirring
  8. waitwas carried out for 5 hours at room temperature
  9. extractionthe mixture was extracted with ethyl acetate
  10. extractionThe aqueous layer was then extracted with ethyl acetate
  11. washwashed with 1N aqueous sodium hydroxide and brine in that order
  12. dry with materialdried over anhydrous sodium sulfate
  13. concentrationThe dried organic layer was concentrated
  14. customthe residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate:methanol=20:1 to 10:1)
  15. additionFractions containing the target compound
  16. concentrationwere concentrated
  17. customto provide a white solid
  18. stirringthe mixture was stirred at room temperature for 1 hour
  19. customThe reaction mixture was then partitioned between ethyl acetate and brine
  20. washThe organic layer was washed with brine
  21. dry with materialdried over anhydrous sodium sulfate
  22. concentrationIt was subsequently concentrated
  23. customThe residue was purified by LC-MS (eluent; acetonitrile-water-trifluoroacetic acid system)
  24. additionFractions containing the target compound
  25. concentrationwere concentrated
  26. customThe residue was partitioned between ethyl acetate and saturated aqueous sodium hydrogencarbonate
  27. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  28. concentrationIt was then concentrated

出典と根拠

ORDレコード
ord-f7446b47e14e4ab5b423a91285931246
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531532B2

反応ノート

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