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Triphenylphosphine → HCID 69085829, 화합물

HRID 2362465
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HRID 2362465 반응식
C(C1C=C([C@@H]2[C@@H:13]([C:14]3C=CC=C(F)C=3)[O:12]C(=O)N2)C=[N:7]C=1)#C.F[C:23]1[CH:28]=[CH:27][C:26]([F:29])=[CH:25][C:24]=1[C@H:30]1[O:34][C:33](=[O:35])[NH:32][C@@H:31]1[C:36]1[CH:37]=[N:38][CH:39]=[C:40]([C:42]#[CH:43])[CH:41]=1.FC1C=C(C=CC=1)C=O.Br[C:54]1[CH:59]=[N:58][CH:57]=[CH:56][N:55]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(N(C(C)C)CC)(C)C>[Pd](Cl)Cl.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cu]I.CN(C)C=O>[C:13]([O-:12])(=[O:34])[CH3:14].[NH4+:7].[F:29][C:26]1[CH:25]=[C:24]([C@H:30]2[O:34][C:33](=[O:35])[NH:32][C@@H:31]2[C:36]2[CH:37]=[N:38][CH:39]=[C:40]([C:42]#[C:43][C:54]3[CH:59]=[N:58][CH:57]=[CH:56][N:55]=3)[CH:41]=2)[CH:23]=[CH:28][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 6

HCID 11776TriphenylphosphineHCID 680093-FluorobenzaldehydeHCID 81531DiisopropylethylamineHCID 6428002-BromopyrazineHCID 86673452HCID 86673452, 화합물HCID 86673456HCID 86673456, 화합물

생성물 2

HCID 517165
Ammonium Acetate
HCID 69085829HCID 69085829, 화합물수율 48%

시약·촉매·용매 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 6102075Dichlorobis(triphenylphosphine)palladium촉매HCID 6228Dimethylformamide용매

실험 절차

(4R,5R)-4-(5-ethynylpyridin-3-yl)-5-(3-fluorophenyl)oxazolidin-2-one (50 mg, 0.177 mmol; prepared in analogous fashion to the preparation of (4R,5R)-5-(2,5-difluorophenyl)-4-(5-ethynylpyridin-3-yl)oxazolidin-2-one starting from 3-fluorobenzaldehyde in place of 2,5-difluorobenzaldehyde), 2-bromopyrazine (31.0 mg, 0.195 mmol), bis(triphenylphosphine) palladium (II) chloride (6.22 mg, 8.86 mmol), triphenylphosphine (9.29 mg, 0.035 mmol), and copper (I) iodide (1.687 mg, 8.86 mmol) were combined in a microwave vial. Dimethylformamide (0.250 mL) and diisopropylethylamine (0.75 mL) were added resulting in a biphasic mixture. Nitrogen was bubbled through the vessel for 10 min, the vessel was capped and the reaction was run at 120° C. for 25 min on a Biotage microwave reactor. The diisopropylethylamine removed in vacuo, the remaining solution was diluted with methanol and the solution was purified via preparative liquid chromatography (Sunfire C18 19×100 mm 5 nm, A=95% H2O/5% Acetonitrile, B=95% Acetonitrile/5% H2O, Modifier 10 mM Ammonium Acetate, 0.00 min=20% B, 8.0 min=100% B, 13.0 min=100% B, Flow rate=25 mL/min) providing (4R,5R)-5-(3-fluorophenyl)-4-(5-(pyrazin-2-ylethynyl)pyridin-3-yl)oxazolidin-2-one (31 mg; 48%) as an amber foam. 1H NMR (500 MHz, CDCl3) δ ppm 8.89 (1H, br. s.), 8.81 (1H, s), 8.63 (1H, d, J=1.53 Hz), 8.57 (1H, d, J=2.44 Hz), 8.52 (1H, br. s.), 7.97 (1H, s), 7.41 (1H, td, J=7.93, 5.49 Hz), 6.94-7.19 (3H, m), 5.61 (1H, br. s.), 5.30 (1H, d, J=7.32 Hz), 4.81 (1H, d, J=7.32 Hz), Mass Spectral Anal. Calcd. for [M+H]+ C20H13FN4O2: 361.1. found 361.2.

후처리

  1. customresulting in a biphasic mixture
  2. customNitrogen was bubbled through the vessel for 10 min
  3. customthe vessel was capped
  4. customThe diisopropylethylamine removed in vacuo
  5. additionthe remaining solution was diluted with methanol
  6. customthe solution was purified via preparative liquid chromatography (Sunfire

출처 및 근거

ORD 기록
ord-79c27586112c409a8d4cbbeed72848f5
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691821B2

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