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Trifluoroacetic acid → HCID 178473812、化合物

HRID 1963958
ノート
印刷プレビュー

反応式

HRID 1963958 の反応式
[Cl:1][C:2]1[C:3]([C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([N:32]([C@H]3CCCNC3)[CH3:33])[N:27]=2)=[CH:4][C:5]([NH:8][C@H:9]2[CH2:14][CH2:13][C@H:12]([NH:15]C(=O)OCC3C=CC=CC=3)[CH2:11][CH2:10]2)=[N:6][CH:7]=1.C(O[C:44](=[O:46])[CH3:45])(=O)C.[C:47](O)([C:49](F)(F)F)=O>[Pd].C(Cl)Cl.CO>[NH2:15][C@H:12]1[CH2:13][CH2:14][C@H:9]([NH:8][C:5]2[CH:4]=[C:3]([C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([NH:32][CH2:33][C@H:49]4[CH2:47][CH2:4][CH2:5][N:6]([C:44](=[O:46])[CH3:45])[CH2:7]4)[N:27]=3)[C:2]([Cl:1])=[CH:7][N:6]=2)[CH2:10][CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 6422Trifluoroacetic acidHCID 7918Acetic AnhydrideHCID 178482137HCID 178482137、化合物

生成物 1

HCID 178473812HCID 178473812、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

A mixture of benzyl trans-4-(5′-chloro-6-((S)-piperidin-3-yl-methylamino)-2,4′-bipyridin-2′-yl-amino)cyclohexylcarbamate (15 mg, 0.027 mmol), DCM (2 mL), TEA (0.011 mL, 0.082 mmol) and acetic anhydride (3.09 μL, 0.033 mmol) was stirred at ambient temperature for 2 hours and the reaction progress was followed by LCMS. The solvent was concentrated off. The reaction mixture flask was flushed with argon, 10% palladium on activated carbon (5 mg, 4.70 μmol) was added and followed by careful addition of MeOH (0.8 mL). The resulting mixture was stirred under hydrogen for 45 minutes at ambient temperature and monitored by LCMS. To the crude reaction mixture was added 2 ml of DCM, filtered and the solvent was concentrated off. The resulting residue was dissolved in 1.0 ml of DMSO, filtered and purified by prep HPLC to give two fractions corresponding to the two title compounds respectively. After lyophilization, 4.0 mg of 1-((R)-3-((2′-(trans-4-aminocyclohexylamino)-5′-chloro-2,4′-bipyridin-6-yl-amino)methyl)piperidin-1-yl)ethanone, was obtained as a TFA salt. LCMS (m/z): 457.2 (MH+), retention time=0.46 min. In addition, 1.0 mg of 1-((R)-3-((2′-(trans-4-aminocyclohexylamino)-2,4′-bipyridin-6-yl-amino)methyl)piperidin-1-yl)ethanone, as TFA salt was also obtained. LCMS (m/z): 423.2 (MH+), retention time=0.45 min. This reaction yielded two products which are separated and purified by HPLC.

後処理

  1. concentrationThe solvent was concentrated off
  2. additionwas added
  3. stirringThe resulting mixture was stirred under hydrogen for 45 minutes at ambient temperature
  4. customTo the crude reaction mixture
  5. filtrationfiltered
  6. concentrationthe solvent was concentrated off
  7. dissolutionThe resulting residue was dissolved in 1.0 ml of DMSO
  8. filtrationfiltered
  9. custompurified by prep HPLC
  10. customto give two fractions corresponding to the two title compounds respectively

出典と根拠

ORDレコード
ord-46238970d4194f40a6f9b11dc82cd8c0
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08415381B2

反応ノート

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