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Trifluoroacetic acid → (R)-6-(3-Amino-3-(trifluoromethyl)pyrrolidin-1-yl)-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

HRID 924102
ノート
印刷プレビュー

反応式

HRID 924102 の反応式
Cl[C:2]1[C:21]([C:22]2[CH:23]=[N:24][CH:25]=[N:26][CH:27]=2)=[CH:20][C:5]([C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][C:16]([F:19])([F:18])[F:17])=[CH:11][CH:10]=2)=[O:7])=[CH:4][N:3]=1.CC([N:32](C([O-])=O)[CH:33]1[CH2:37][N:36](C(F)(F)F)[CH2:35][CH2:34]1)(C)C.CCN(C(C)C)C(C)C.C(O)([C:56]([F:59])([F:58])[F:57])=O>CC(O)C.CCOC(C)=O.C(Cl)Cl.CC#N>[NH2:32][C@:33]1([C:56]([F:59])([F:58])[F:57])[CH2:34][CH2:35][N:36]([C:2]2[C:21]([C:22]3[CH:23]=[N:24][CH:25]=[N:26][CH:27]=3)=[CH:20][C:5]([C:6]([NH:8][C:9]3[CH:14]=[CH:13][C:12]([O:15][C:16]([F:19])([F:18])[F:17])=[CH:11][CH:10]=3)=[O:7])=[CH:4][N:3]=2)[CH2:37]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

9

反応物 4

HCID 6422Trifluoroacetic acidHCID 81531DiisopropylethylamineHCID 53432656N-tert-butyl-N-[1-(trifluoromethyl)pyrrolidin-3-yl]carbamateHCID 722034246-Chloro-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

生成物 1

HCID 118195289(R)-6-(3-Amino-3-(trifluoromethyl)pyrrolidin-1-yl)-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

試薬・触媒・溶媒 4

HCID 3776Isopropanol溶媒HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒2 回

反応条件

温度
140 °C

実験手順

6-Chloro-5-(pyrimidin-5-yl)-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 223.1, 150 mg, 0.380 mmol) was suspended in iPrOH (0.6 mL). tert-Butyl[3-(trifluoromethylpyrrolidine-3-yl)]carbamate (193 mg, 0.760 mmol) and DIPEA (0.265 mL, 1.520 mmol) were added at RT. The pink/red suspension was stirred at 140° C. for 22 h. The orange reaction solution was diluted with EtOAc (50 mL) then washed with a 2 N citric acid solution (20 mL) and water (3×20 mL). Aq. phases were back-extracted with EtOAc (40 mL). The combined organic phases were dried over Na2SO4, filtered, and the solvent was evaporated off under reduced pressure to give a crude product that was purified by flash chromatography (RediSep® Silica gel column, 40 g, DCM/EtOAc 7:3). The resulting intermediate (135 mg, 0.22 mmol) was suspended in DCM (2 mL). TFA (0.679 mL, 8.82 mmol) was added at RT and the resulting light yellow solution was stirred for 2 h at RT. The RM was diluted with EtOAc (50 mL), washed with an aq. sat. solution of NaHCO3 (2×20 mL) and water (2×20 mL). Aq. phases were back-extracted with EtOAc (40 mL). The combined organic phases were dried over Na2SO4, filtered, and the solvent was evaporated off under reduced pressure to give a crude product that was suspended in MeCN (2 mL). The white suspension was stirred for 30 min at RT then filtered. The solid was washed with MeCN (2 mL) and dried under reduced pressure to give the title product as a white solid. HPLC (Condition 10) tR=5.748 min, UPLC-MS (Condition 3) tR=1.03 min, m/z=513.1 [M+H]+; 1H-NMR (400 MHz, DMSO-d6) δ ppm 1.75-1.85 (m, 1H) 1.96-2.08 (m, 1H) 2.24-2.35 (m, 2H) 3.13-3.26 (m, 2H) 3.36-3.52 (m, 2H) 7.36 (d, J=8.99 Hz, 2H) 7.86 (d, J=8.99 Hz, 2H) 8.14 (d, J=2.35 Hz, 1H) 8.81 (d, J=2.35 Hz, 1H) 8.92 (s, 2H) 9.22 (s, 1H) 10.22 (s, 1H).

後処理

  1. washthen washed with a 2 N citric acid solution (20 mL) and water (3×20 mL)
  2. extractionAq. phases were back-extracted with EtOAc (40 mL)
  3. dry with materialThe combined organic phases were dried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent was evaporated off under reduced pressure
  6. customto give a crude product that
  7. customwas purified by flash chromatography (RediSep® Silica gel column, 40 g, DCM/EtOAc 7:3)
  8. stirringthe resulting light yellow solution was stirred for 2 h at RT
  9. washwashed with an aq. sat. solution of NaHCO3 (2×20 mL) and water (2×20 mL)
  10. extractionAq. phases were back-extracted with EtOAc (40 mL)
  11. dry with materialThe combined organic phases were dried over Na2SO4
  12. filtrationfiltered
  13. customthe solvent was evaporated off under reduced pressure
  14. customto give a crude product that
  15. stirringThe white suspension was stirred for 30 min at RT
  16. filtrationthen filtered
  17. washThe solid was washed with MeCN (2 mL)
  18. customdried under reduced pressure

出典と根拠

ORDレコード
ord-7bdc3c9e44d14861beb1f38dbd68e3dc
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278981B2

反応ノート

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