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Acetic Acid → HCID 178521010, 화합물

HRID 931208
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HRID 931208 반응식
Cl.Cl.[NH2:3][C:4]1[CH:5]=[CH:6][C:7]([N:11]2[CH2:16][CH2:15][CH2:14][C@@H:13]([C:17]([N:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)=[O:18])[CH2:12]2)=[N:8][C:9]=1[NH2:10].C(O)(=O)C.C(N(CC)CC)C.[CH:35]1([C:38]2[N:43]=[C:42]([C:44](=N)OCC)[CH:41]=[CH:40][N:39]=2)[CH2:37][CH2:36]1>C(O)C>[CH:35]1([C:38]2[N:43]=[C:42]([C:44]3[NH:10][C:9]4=[N:8][C:7]([N:11]5[CH2:16][CH2:15][CH2:14][C@@H:13]([C:17]([N:19]6[CH2:23][CH2:22][CH2:21][CH2:20]6)=[O:18])[CH2:12]5)=[CH:6][CH:5]=[C:4]4[N:3]=3)[CH:41]=[CH:40][N:39]=2)[CH2:37][CH2:36]1
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참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 8471TriethylamineHCID 89854051(R)-(1-(5,6-Diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochlorideHCID 89854162Ethyl 2-cyclopropylpyrimidine-4-carbimidate

생성물 1

HCID 178521010HCID 178521010, 화합물

시약·촉매·용매 1

HCID 702
Ethanol
용매
2회

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온도
40 °C

실험 절차

To a suspension of (R)-(1-(5,6-diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride (1.0 g, 2.76 mmol) and acetic acid (2.5 mL, 43.4 mmol) in ethanol (7 mL) was added triethylamine (1.5 mL, 10.8 mmol). A solution of ethyl 2-cyclopropylpyrimidine-4-carbimidate (530 mg, 2.77 mmol) in ethanol (3 mL) was added. The reaction mixture was heated at reflux for 30 min, then was cooled. The solvent was removed under reduced pressure and ethyl acetate (100 mL) was added to the residue followed by water (10 mL) and a saturated aqueous solution of ammonium chloride (50 mL). The layers were separated and the organics were washed with a saturated aqueous solution of sodium bicarbonate (75 mL) and brine (50 mL), dried over magnesium sulfate, filtered and concentrated under reduced pressure. To the resulting residue was added dichloromethane (4 mL) and methyl tert-butyl ether (35 mL). The mixture was stirred at 40° C. unit it was homogeneous. The solution was cooled to room temperature and stirred for 18 h. The resulting solids were filtered and rinsed with ether to afford the title compound. 1H NMR (400 MHz, CDCl3) δ 1.10-1.17 (m, 2H) 1.18-1.23 (m, 2H), 1.57-1.70 (m, 1H) 1.82-2.05 (m, 7H) 2.27-2.34 (m, 1H) 2.63-2.72 (m, 1H) 2.97-3.07 (m, 1H) 3.14-3.22 (m, 1H) 3.43-3.54 (m, 3H) 3.58-3.67 (m, 1H) 4.37 (d, 1H) 4.53 (d, 1H) 6.76 (d, 1H) 7.95 (m, 2H) 8.67 (d, 1H) 10.46 (br, 1H). MS (ES+) (M+H) 418.5; LCMS retention time 2.72 min (Method L).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 30 min
  3. temperaturewas cooled
  4. customThe solvent was removed under reduced pressure and ethyl acetate (100 mL)
  5. additionwas added to the residue
  6. customThe layers were separated
  7. washthe organics were washed with a saturated aqueous solution of sodium bicarbonate (75 mL) and brine (50 mL)
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. additionTo the resulting residue was added dichloromethane (4 mL) and methyl tert-butyl ether (35 mL)
  12. temperatureThe solution was cooled to room temperature
  13. stirringstirred for 18 h
  14. filtrationThe resulting solids were filtered
  15. washrinsed with ether

출처 및 근거

ORD 기록
ord-e8b7733966624d09bfc04162aaefadd3
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296745B2

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