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Sodium Bicarbonate → 2-(3-{[2,2-Difluoro-2-(4-fluoronaphthyl)ethyl]amino]-6-chloro-2-fluorophenyl)ethanol

HRID 2184205
ノート
印刷プレビュー

反応式

HRID 2184205 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=O)[C:10]([F:23])([F:22])[C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([F:21])=[CH:13][CH:12]=2)=[C:4]([F:25])[C:3]=1[CH2:26][CH2:27][OH:28].B.C1COCC1.C([O-])(O)=O.[Na+]>C1COCC1.O>[F:23][C:10]([F:22])([C:11]1[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:14]([F:21])=[CH:13][CH:12]=1)[CH2:9][NH:8][C:5]1[C:4]([F:25])=[C:3]([CH2:26][CH2:27][OH:28])[C:2]([Cl:1])=[CH:7][CH:6]=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

6

反応物 3

HCID 516892Sodium BicarbonateHCID 2723981Borane;tetrahydrofuranHCID 22475325N-[4-chloro-2-fluoro-3-(2-hydroxyethyl)phenyl]-2,2-difluoro-2-(4-fluoronaphthyl)acetamide

生成物 1

HCID 224753262-(3-{[2,2-Difluoro-2-(4-fluoronaphthyl)ethyl]amino]-6-chloro-2-fluorophenyl)ethanol収率 44%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
77.5 °C

実験手順

To a solution of N-[4-chloro-2-fluoro-3-(2-hydroxyethyl)phenyl]-2,2-difluoro-2-(4-fluoronaphthyl)acetamide (1.9 g, 4.6 mmol), as prepared in the preceding step, in THF (19 mL) at 0° C. was added dropwise a solution of BH3.THF complex (19.4 mL, 19.4 mmol, 1.0 M in THF) over a period of 20 minutes, and the reaction mixture continued to stir until the ice bath expired. The mixture was then heated at reflux in an oil bath at 75 to 80° C. for 3 hours, and continued to stir at ambient temperature overnight. A solution of NaHCO3 (1.63 g, 19.4 mmol) in H2O (20 mL) was added, the THF was evaporated, and the resulting mixture was extracted with DCM twice. The extracts were combined, washed with H2O and brine, dried over Na2SO4, concentrated, and flash chromatographed on silica gel eluting with EtOAc/DCM (0, 1, 1.5%) to give the title compound (805 mg, 44% yield) as a white solid. 1H-NMR (400 MHz, CDCl3) δ 8.24-8.19 (m, 2H), 7.70-7.61 (m, 3H), 7.14 (t, J=9.3 Hz, 1H), 6.90 (dd, J=8.7, 1.6 Hz, 1H), 6.42 (t, J=8.9 Hz, 1H), 4.22-4.16 (m, 1H), 4.00 (dt, J=13.4, 6.8 Hz, 2H), 3.82 (dd, J=12.1, 6.4 Hz, 2H), 3.02 (dt, J=6.8, 2.3 Hz, 2H), 1.39 (br s, 1H). Mass spectrum (LCMS, ESI) calc'd for C20H17ClF4NO (M+H): 398.1. Found: 398.3.

後処理

  1. temperatureThe mixture was then heated
  2. customthe THF was evaporated
  3. extractionthe resulting mixture was extracted with DCM twice
  4. washwashed with H2O and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customflash chromatographed on silica gel eluting with EtOAc/DCM (0, 1, 1.5%)

出典と根拠

ORDレコード
ord-e52b8fa468ff47ec92520c695677b3bc
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06900231B2

反応ノート

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