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1-Bromo-3-chloropropane → 1-[3-(4-Butylpiperidin-1-yl)propyl]-7-fluoro-1h-quinolin-2-one

HRID 969428
ノート
印刷プレビュー

反応式

HRID 969428 の反応式
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1.[H-].[Na+].Br[CH2:16][CH2:17][CH2:18]Cl.C([O-])([O-])=O.[K+].[K+].[CH2:26]([CH:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)[CH2:27][CH2:28][CH3:29]>CCOCC.O.CCOC(C)=O.CN(C=O)C>[CH2:26]([CH:30]1[CH2:35][CH2:34][N:33]([CH2:16][CH2:17][CH2:18][N:9]2[C:10]3[C:5](=[CH:4][CH:3]=[C:2]([F:1])[CH:11]=3)[CH:6]=[CH:7][C:8]2=[O:12])[CH2:32][CH2:31]1)[CH2:27][CH2:28][CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 132838674-ButylpiperidineHCID 190675757-Fluoroquinolin-2(1H)-one

生成物 1

HCID 179561101-[3-(4-Butylpiperidin-1-yl)propyl]-7-fluoro-1h-quinolin-2-one収率 11%

試薬・触媒・溶媒

4
HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A 4 mL vial was charged with 7-fluoro-1H-quinolin-2-one (0.032 g, 0.19 mmol), NaH (60% in oil, 8.7 mg, 0.21 mmol) and dry DMF (2.5 mL). The mixture was shaken at rt for 1 h and then 1-bromo-3-chloropropane (20 IlI, 0.19 mmol) was added and the reaction was shaken overnight shaken at rt overnight. The mixture was then diluted with ether (25 mL) and washed water (15 mL), the ether phase was washed with water (15 mL) and brine (15 mL). The organic phase was dried over Na2SO4, and concentrated under reduced pressure. The oily residue was diluted with CH3CN (2 mL) and to the resulting solution was added: KI (0.050 g, 0.30 mmol), K2CO3 (0.041 g, 0.30 mmol) and 4-butylpiperidine (0.028 g, 0.20 mmol). The mixture was shaken at 50° C. for 72 h and then poured onto The compound EtOAc (25 mL) and water (15 mL). The water phase was extracted (2×25 mL) and the combined organic phase was dried over Na2SO4, and concentrated under reduced pressure. The residue was purified by flash CC (SiO2; EtOAc/MeOH 4:1) followed by prep RP-HPLC to give the title compound (7.0 mg, 11%). 1H NMR (CD3OD) δ 7.89 (d, J=9.6 Hz, 1H), 7.73 (dd, J=6.2, 8.6 Hz, 1H), 7.47 (dd, J=2.4, 11.6 Hz, 1H), 7.08 (dt, J=2.4, 8.6 Hz, 1H), 6.60 (d J=9.6 Hz, 1H), 4.33 (t, J=7.6 Hz, 2 H), 2.98-2.00 (m, 2H), 2.50-2.42 (m, 2H), 2.05-1.86 (m, 4H), 1.55-1.64 (m, 2H), 1.36-1.15 (m, 9H), 0.90 (t, J=6.8 Hz); 13C NMR (CD3OD) δ 164.7 (d, J=248), 163.2, 140.9 (br) 139.9, 131.4 (d, J=10 Hz), 119.3 (d, J=3 Hz), 118.1 (br), 110.6 (d, J=23 Hz), 101.6 (d, J=28 Hz), 55.5, 53.9, 41.0, 36.8, 35.6, 31.9, 28.9, 24.5, 22.7, 13.2; HPLC-MS (ammonium acetate) [M+H]+=345.3

後処理

  1. stirringthe reaction was shaken overnight
  2. stirringshaken at rt overnight
  3. washwashed water (15 mL)
  4. washthe ether phase was washed with water (15 mL) and brine (15 mL)
  5. dry with materialThe organic phase was dried over Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. additionThe oily residue was diluted with CH3CN (2 mL) and to the resulting solution
  8. additionwas added
  9. stirringThe mixture was shaken at 50° C. for 72 h
  10. extractionThe water phase was extracted (2×25 mL)
  11. dry with materialthe combined organic phase was dried over Na2SO4
  12. concentrationconcentrated under reduced pressure
  13. customThe residue was purified by flash CC (SiO2; EtOAc/MeOH 4:1)

出典と根拠

ORDレコード
ord-65f83fd449044321bcdc02d155da39a5
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07307075B2

反応ノート

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