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Hydrochloric Acid → tert-Butyl 3-(4-((4-(2-(3-(2-amino-2-oxoethyl)pyridin-2-yl)ethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate

HRID 1485288
ノート
印刷プレビュー

反応式

HRID 1485288 の反応式
O[N:2]1C2C=CC=CC=2N=N1.CCN=C=NCCCN(C)C.Cl.Cl.C(N(CC)C(C)C)(C)C.[C:33]([O:37][C:38]([N:40]1[CH2:45][CH2:44][CH2:43][CH:42]([C:46]2[CH:51]=[CH:50][C:49]([NH:52][C:53]3[N:58]=[C:57]([CH2:59][CH2:60][C:61]4[C:66]([CH2:67][C:68](O)=[O:69])=[CH:65][CH:64]=[CH:63][N:62]=4)[C:56]([C:71]([F:74])([F:73])[F:72])=[CH:55][N:54]=3)=[CH:48][CH:47]=2)[CH2:41]1)=[O:39])([CH3:36])([CH3:35])[CH3:34].C(=O)([O-])[O-].[NH4+].[NH4+]>CN(C=O)C>[NH2:2][C:68](=[O:69])[CH2:67][C:66]1[C:61]([CH2:60][CH2:59][C:57]2[C:56]([C:71]([F:73])([F:74])[F:72])=[CH:55][N:54]=[C:53]([NH:52][C:49]3[CH:48]=[CH:47][C:46]([CH:42]4[CH2:43][CH2:44][CH2:45][N:40]([C:38]([O:37][C:33]([CH3:35])([CH3:34])[CH3:36])=[O:39])[CH2:41]4)=[CH:51][CH:50]=3)[N:58]=2)=[N:62][CH:63]=[CH:64][CH:65]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 313Hydrochloric Acid2 回HCID 757711-Hydroxybenzotriazole2 回HCID 81531Diisopropylethylamine2 回HCID 517111Ammonium Carbonate2 回HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride2 回
HCID 68282857
2-(2-(2-(2-((4-(1-(tert-Butoxycarbonyl)piperidin-3-yl)phenyl)amino)-5-(trifluoromethyl)pyrimidin-4-yl)ethyl)pyridin-3-yl)acetic acid

生成物 1

HCID 71209278tert-Butyl 3-(4-((4-(2-(3-(2-amino-2-oxoethyl)pyridin-2-yl)ethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperidine-1-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-Hydroxybenzotriazole (20 mg, 0.15 mmol), EDCl.HCl (32 mg, 0.17 mmol) and N,N-diisopropylethylamine (45 μL, 0.26 mmol) were added to a solution of 2-(2-(2-(2-((4-(1-(tert-butoxycarbonyl)piperidin-3-yl)phenyl)amino)-5-(trifluoromethyl)pyrimidin-4-yl)ethyl)pyridin-3-yl)acetic acid (1149) (29 mg, 0.051 mmol) in dry DMF (5 mL) under an atmosphere of nitrogen. Ammonium carbonate (50 mg, 0.52 mmol) was added in one portion after 10 minutes then stirring was continued at room temperature for 17 hours. Further portions of 1-hydroxybenzotriazole (20.0 mg, 0.15 mmol), EDCl.HCl (32 mg, 0.17 mmol) and N,N-diisopropylethylamine (45 μL, 0.26 mmol) were added, then ammonium carbonate (50 mg, 0.52 mmol) was added in one portion after 10 min. The resulting solution was stirred at 25° C. for 24 hours. The volatiles were removed in vacuo and the residue was partitioned between ethyl acetate (I0 mL) and saturated sodium hydrogen carbonate (10 mL). The aqueous layer was extracted with ethyl acetate (2×10 mL) then the combined organic layers were washed with brine (10 mL), dried (MgSO4) and evaporated to dryness. The residue was chromatographed (Biotage Isolera: 10 g silica cartridge, 0-100% EtOAc/petroleum benzine 40-60° C. then 10 g silica cartridge, 50-100% EtOAc/petroleum benzine 40-60° C.) to give the title compound (I150) (0.023 g, 77%) as a white solid; 1H NMR (400 MHz, CDCl3) δ 8.49 (s, 1H), 8.46 (dd, J=4.8, 1.6 Hz, 1H), 7.77 (br s, 1H), 7.57-7.44 (m, 3H), 7.19 (d, J=8.5 Hz, 2H), 7.14 (dd, J=7.6, 4.8 Hz, 1H), 5.63 (d, J=22.0 Hz, 2H), 4.35-3.96 (m), 3.67 (s, 2H), 3.41-3.33 (m, 2H), 3.27 (t, J=6.9 Hz, 2H), 2.83-2.58 (m, 3H), 2.01-1.99 (m, 1H), 1.80-1.71 (m, 1H), 1.68 (s, 3H), 1.65-1.52 (m, 2H), 1.46 (s, 9H).

後処理

  1. stirringThe resulting solution was stirred at 25° C. for 24 hours
  2. customThe volatiles were removed in vacuo
  3. customthe residue was partitioned between ethyl acetate (I0 mL) and saturated sodium hydrogen carbonate (10 mL)
  4. extractionThe aqueous layer was extracted with ethyl acetate (2×10 mL)
  5. washthe combined organic layers were washed with brine (10 mL)
  6. dry with materialdried (MgSO4)
  7. customevaporated to dryness
  8. customThe residue was chromatographed (Biotage Isolera

出典と根拠

ORDレコード
ord-a17db31fdd724157aa98052f1b52cb9e
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09421205B2

反応ノート

読み込み中…

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