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8-Chloroquinoline → 2-(Quinolin-8-ylamino)cyclohexanecarboxylic acid

HRID 352567
ノート
印刷プレビュー

反応式

HRID 352567 の反応式
Cl.[NH2:2][C@H:3]1[CH2:8][CH2:7][CH2:6][CH2:5][C@H:4]1[C:9]([O:11]CC)=[O:10].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.CC(C)([O-])C.[Na+].Cl[C:67]1[CH:68]=[CH:69][CH:70]=[C:71]2[C:76]=1[N:75]=[CH:74][CH:73]=[CH:72]2>C(OCC)C.C(OCC)(=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[N:75]1[C:76]2[C:71](=[CH:70][CH:69]=[CH:68][C:67]=2[NH:2][CH:3]2[CH2:8][CH2:7][CH2:6][CH2:5][CH:4]2[C:9]([OH:11])=[O:10])[CH:72]=[CH:73][CH:74]=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 691398-ChloroquinolineHCID 634876Binap, (A+-)-HCID 2724641ethyl (1R,2S)-2-aminocyclohexane-1-carboxylate hydrochlorideHCID 23676156Sodium t-butoxide

生成物 1

HCID 235102622-(Quinolin-8-ylamino)cyclohexanecarboxylic acid収率 15.1%

試薬・触媒・溶媒 4

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒
HCID 3283Diethyl Ether溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

To an oven-dried Schlenk flask that was evacuated and backfilled with argon was added 726 mg (3.68 mmol) of ethyl cis-2-amino-1-cyclohexanecarboxylate HCl salt, 56 mg (0.06 mmol, 2 mol % Pd) of Pd2(dba)3, 77 mg (0.12 mmol, 4 mol %) of rac-BINAP, 881 mg (9.17 mmol) of sodium tert-butoxide, 500 mg (3.06 mmol) of 8-chloroquinoline, and 7.5 mL of toluene. The flask was sealed with a glass stopper and an argon balloon replacing the source. The reaction mixture was then heated to 90° C. and stirred at that temperature for 17 hours. The mixture was allowed to cool to room temperature, taken up in diethyl ether (35 mL), washed three times with saturated brine (30 mL), dried over magnesium sulfate, and concentrated to provide the crude reaction mixture. The crude mixture was re-dissolved in ethyl acetate, partitioned between ethyl acetate and 1N HCl, dried over magnesium sulfate and concentrated to provide 125 mg (15%) of 2-(quinolin-8-ylamino)cyclohexanecarboxylic acid with both cis and trans isomers in 1:1 ratio. Confirmed by 1H NMR.

後処理

  1. customTo an oven-dried Schlenk flask that was evacuated
  2. customThe flask was sealed with a glass stopper
  3. temperatureto cool to room temperature
  4. washwashed three times with saturated brine (30 mL)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customto provide the crude
  8. customreaction mixture
  9. custompartitioned between ethyl acetate and 1N HCl
  10. dry with materialdried over magnesium sulfate
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-b903d47a843f4c0393bc6e2b6af1e091
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06747053B2

反応ノート

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