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Trifluoroacetic acid → methyl 4-[[1-[4-[N'-(2-methylphenyl)ureido]phenylacetyl]-(2S)-pyrrolidinyl]methoxy]cyclohexanecarboxylate

HRID 354463
ノート
印刷プレビュー

反応式

HRID 354463 の反応式
C(O[C:6]([N:8]1[CH2:12][CH2:11][CH2:10][CH:9]1[CH2:13][O:14][CH:15]1[CH2:20][CH2:19][CH:18]([C:21]([O:23][CH3:24])=[O:22])[CH2:17][CH2:16]1)=[O:7])(C)(C)C.[C:25]([OH:31])(C(F)(F)F)=O.[CH:32]1[CH:33]=[CH:34][C:35]2N(O)N=[N:38][C:36]=2[CH:37]=1.[CH2:42](N(CC)CC)C.CCN=C=N[CH2:54][CH2:55][CH2:56][N:57](C)C.Cl.[CH2:61]1[CH2:65]O[CH2:63][CH2:62]1>C(Cl)Cl.CC#N>[CH3:42][C:35]1[CH:34]=[CH:33][CH:32]=[CH:37][C:36]=1[NH:38][C:25](=[O:31])[NH:57][C:56]1[CH:55]=[CH:54][C:61]([CH2:65][C:6]([N:8]2[CH2:12][CH2:11][CH2:10][C@H:9]2[CH2:13][O:14][CH:15]2[CH2:16][CH2:17][CH:18]([C:21]([O:23][CH3:24])=[O:22])[CH2:19][CH2:20]2)=[O:7])=[CH:62][CH:63]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 6422Trifluoroacetic acidHCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 23512198HCID 23512198、化合物

生成物 1

HCID 69333464
methyl 4-[[1-[4-[N'-(2-methylphenyl)ureido]phenylacetyl]-(2S)-pyrrolidinyl]methoxy]cyclohexanecarboxylate
収率 78%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of methyl 4-[(1-tert-butoxycarbonyl-2-pyrrolidinyl)methoxy]cyclohexane carboxylate (450 mg, 1.3 mmol) in CH2Cl2 (5.0 ml) was added TFA (5.0 ml) at 0° C. The reaction mixture was stirred at room temperature for 0.5 hr. The mixture was concentrated in vacuo. Sat. NaHCO3 was added to the residue, and extracted with CH2Cl2. The extract was washed with brine, dried over Na2SO4, and concentrated in vacuo. The crude product was used to the subsequent reaction without further purification. To a stirred solution of the crude product, 4-[N′-(2-methylphenyl)uredio]phenylacetic acid (375 mg, 1.3 mmol), HOBt (178 mg, 1.3 mmol), and triethylamine (550 ml, 3.9 mmol) in THF (6.0 ml) and MeCN (6.0 ml) was added EDC.HCl (380 mg, 1.9 mmol) at 0° C. The reaction mixture was stirred at room temperature for 16 hr, and concentrated in vacuo. Water was added to the residue, and extracted with EtOAc. The extract was washed with sat. NaHCO3, 2-M citric acid, and sat. NaHCO3, then dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel with n-hexane-EtOAc (1:6, v/v) as eluent to give methyl 4-[[1-[4-[N′-(2-methylphenyl)ureido]phenylacetyl]-(2S)-pyrrolidinyl]methoxy]cyclohexanecarboxylate (520 mg, 78%) as a colorless oil. 1H-NMR (CDCl3) δ1.30-2.40 (m, 13H), 2.21 (s, 3H), 3.30-3.80 (m, 7H), 3.65 (s, 3H), 4.10-4.30 (m, 1H), 6.90-7.20 (m, 8H), 7.40-7.70 (m, 2H).

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. additionSat. NaHCO3 was added to the residue
  3. extractionextracted with CH2Cl2
  4. washThe extract was washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe crude product was used to the subsequent reaction without further purification
  8. stirringThe reaction mixture was stirred at room temperature for 16 hr
  9. concentrationconcentrated in vacuo
  10. additionWater was added to the residue
  11. extractionextracted with EtOAc
  12. washThe extract was washed with sat. NaHCO3, 2-M citric acid, and sat. NaHCO3
  13. dry with materialdried over Na2SO4
  14. concentrationconcentrated in vacuo
  15. customThe residue was purified by column chromatography on silica gel with n-hexane-EtOAc (1:6, v/v) as eluent

出典と根拠

ORDレコード
ord-6bc23836fc23479ca7fecb0a813b5a1e
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06756378B2

反応ノート

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