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Phenylacetylene → (4R,5R)-5-(2,5-Difluorophenyl)-4-(5-fluoro-2-(phenylethynyl)pyridin-4-yl)oxazolidin-2-one

HRID 2362459
ノート
印刷プレビュー

反応式

HRID 2362459 の反応式
Br[C:2]1[CH:7]=[C:6]([C@@H:8]2[C@@H:12]([C:13]3[CH:18]=[C:17]([F:19])[CH:16]=[CH:15][C:14]=3[F:20])[O:11][C:10](=[O:21])[NH:9]2)[C:5]([F:22])=[CH:4][N:3]=1.[C:23]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)#[CH:24].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(N(CC)CC)C.[Cu]I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[F:20][C:14]1[CH:15]=[CH:16][C:17]([F:19])=[CH:18][C:13]=1[C@H:12]1[O:11][C:10](=[O:21])[NH:9][C@@H:8]1[C:6]1[C:5]([F:22])=[CH:4][N:3]=[C:2]([C:24]#[C:23][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:7]=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 10821PhenylacetyleneHCID 11776TriphenylphosphineHCID 86673438(4R,5R)-4-(2-bromo-5-fluoropyridin-4-yl)-5-(2,5-difluorophenyl)oxazolidin-2-one

生成物 1

HCID 69081526(4R,5R)-5-(2,5-Difluorophenyl)-4-(5-fluoro-2-(phenylethynyl)pyridin-4-yl)oxazolidin-2-one収率 16%

試薬・触媒・溶媒 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 178418476HCID 178418476、化合物触媒
HCID 8471Triethylamine溶媒

実験手順

In a 1 mL scint vial, a suspension of optically-enriched (4R,5R)-4-(2-bromo-5-fluoropyridin-4-yl)-5-(2,5-difluorophenyl)oxazolidin-2-one (20 mg, 0.054 mmol), and ethynylbenzene (0.014 mL, 0.129 mmol) in triethyl amine (1.5 mL) was purged with nitrogen for 30 min. Triphenylphosphine (3.7 mg, 0.014 mmol) was added and the suspension stirred for 5 min. To this was added copper (I) iodide (0.408 mg, 2.144 μmol), and bis(triphenylphosphine)palladium(II) chloride (1.8 mg, 2.6 μmol). The vial was purged with nitrogen for an additional 5 min, capped, and immersed in a 90° C. bath for 5 h. The reaction was cooled to room temperature and concentrated. The resulting residue was dissolved in dichloromethane and poured into water. The mixture was diluted with ethyl acetate, washed with water, brine, dried over magnesium sulfate, and concentrated. The material was purified first by reversed phase HPLC (TFA/MeOH/sunfire column) to give an optically enriched mixture of regioisomers. The material was further purified by chiral prep HPLC (Chiralpak AD, A=heptane/0.1% DEA, B=ethanol, 40%→60% over 35 min) to give the title compound (3.4 mg). 1H NMR (CDCl3) δ: 8.52 (d, J=0.9 Hz, 1H), 7.75 (d, J=5.8 Hz, 1H), 7.63 (dd, J=7.3, 2.1 Hz, 2H), 7.38-7.44 (m, 3H), 7.23-7.27 (m, 1H), 7.11-7.17 (m, 2H), 5.79 (br. s., 1H), 5.64 (d, J=5.5 Hz, 1H), 5.08 (d, J=5.5 Hz, 1H). 1H NMR (CDCl3) δ: 8.51 (d, J=0.9 Hz, 1H), 7.73 (d, J=5.5 Hz, 1H), 7.63 (dd, J=7.6, 1.8 Hz, 2H), 7.39-7.46 (m, 3H), 7.23-7.27 (m, 1H), 7.10-7.16 (m, 2H), 5.95 (br. s., 1H), 5.61 (d, J=5.5 Hz, 1H), 5.13 (d, J=5.8 Hz, 1H). Mass spec.: 395.2 (MH)+.

後処理

  1. customwas purged with nitrogen for 30 min
  2. customThe vial was purged with nitrogen for an additional 5 min
  3. customcapped
  4. customimmersed in a 90° C.
  5. customfor 5 h
  6. concentrationconcentrated
  7. dissolutionThe resulting residue was dissolved in dichloromethane
  8. additionpoured into water
  9. additionThe mixture was diluted with ethyl acetate
  10. washwashed with water, brine
  11. dry with materialdried over magnesium sulfate
  12. concentrationconcentrated
  13. customThe material was purified first by reversed phase HPLC (TFA/MeOH/sunfire column)
  14. customto give
  15. additionan optically enriched mixture of regioisomers
  16. customThe material was further purified by chiral prep HPLC (Chiralpak AD
  17. customover 35 min

出典と根拠

ORDレコード
ord-7e9d7dbc848042b3be8dbe3083c3f700
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08691821B2

反応ノート

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