ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Tetrahydrofuran → (4S,5R)-5-(3,5-Difluorophenyl)-3-{[2-(3-fluoroazetidin-1-yl)-5-(5-isopropyl-2-methoxypyridin-3-yl)pyrimidin-4-yl]methyl}-4-methyl-1,3-oxazolidin-2-one

HRID 531273
ノート
印刷プレビュー

反応式

HRID 531273 の反応式
C1COCC1.Br[C:7]1[C:8]([CH2:18][N:19]2[C@@H:23]([CH3:24])[C@@H:22]([C:25]3[CH:30]=[C:29]([F:31])[CH:28]=[C:27]([F:32])[CH:26]=3)[O:21][C:20]2=[O:33])=[N:9][C:10]([N:13]2[CH2:16][CH:15]([F:17])[CH2:14]2)=[N:11][CH:12]=1.[CH:34]([C:37]1[CH:38]=[C:39](B(O)O)[C:40]([O:43][CH3:44])=[N:41][CH:42]=1)([CH3:36])[CH3:35].C([O-])([O-])=O.[K+].[K+]>[Pd](Cl)Cl.C(P(C(C)(C)C)[C-]1C=CC=C1)(C)(C)C.[C-]1(P(C(C)(C)C)C(C)(C)C)C=CC=C1.[Fe+2].O>[F:32][C:27]1[CH:26]=[C:25]([C@H:22]2[O:21][C:20](=[O:33])[N:19]([CH2:18][C:8]3[C:7]([C:39]4[C:40]([O:43][CH3:44])=[N:41][CH:42]=[C:37]([CH:34]([CH3:36])[CH3:35])[CH:38]=4)=[CH:12][N:11]=[C:10]([N:13]4[CH2:16][CH:15]([F:17])[CH2:14]4)[N:9]=3)[C@H:23]2[CH3:24])[CH:30]=[C:29]([F:31])[CH:28]=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

7

反応物 4

HCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 90009148(4S,5R)-3-{[5-bromo-2-(3-fluoroazetidin-1-yl)pyrimidin-4-yl]methyl}-5-(3,5-difluorophenyl)-4-methyl-1,3-oxazolidin-2-one2 回HCID 900091535-Isopropyl-2-methoxypyridin-3-ylboronic acid

生成物 1

HCID 72192440
(4S,5R)-5-(3,5-Difluorophenyl)-3-{[2-(3-fluoroazetidin-1-yl)-5-(5-isopropyl-2-methoxypyridin-3-yl)pyrimidin-4-yl]methyl}-4-methyl-1,3-oxazolidin-2-one

試薬・触媒・溶媒 2

HCID 178454861HCID 178454861、化合物触媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

1,1′-Bis(di-tert-butylphosphino)ferrocene palladium dichloride (25.07 mg, 0.038 mmol) was added to a degassed THF (15 mL)/Water (3 mL) solution of (4S,5R)-3-{[5-bromo-2-(3-fluoroazetidin-1-yl)pyrimidin-4-yl]methyl}-5-(3,5-difluorophenyl)-4-methyl-1,3-oxazolidin-2-one (INTERMEDIATE 15, 200 mg, 0.385 mmol), 5-isopropyl-2-methoxypyridin-3-ylboronic acid (128 mg, 0.462 mmol) and K2CO3 (159 mg, 1.154 mmol). After further de-gassing with N2 and vacuum, the reaction was heated for 1 h at 50° C. LCMS showed complete conversion to product. The reaction was diluted with 50 mL ethyl acetate and poured into 100 mL sat′d NH4Cl soln. The ethyl acetate layer was washed with brine (100 mL) filtered through a 20 g plug of sodium sulfate, eluting with 50 mL ethyl acetate. The filtrate was concentrated prior to purification with an X-Bridge 21.2×150 mm RP column. The sample was loaded in 7:3:1 CH3CN/water/DMSO (5 mL), after which a 10-100% acetonitrile/water (0.1% NH4OH) linear gradient at 15 mL/minutes over 20 minutes was run. The product of interest eluted in 80% portion of above gradient. Pure fractions (rich cut; impure discarded) were concentrated and lyophilized to give product as a white solid. LCMS (M+H)+: 528.5. 1H NMR (500 MHz, CDCl3): δ 8.15 (s, 1H), 8.10 (d, J=2.1 Hz, 1H), 7.35 (d, J=2.1 Hz, 1H), 6.84 (m, 3H), 5.52 (m, 1.5H), 5.42 (m, 0.5H), 4.64 (d, J=17.3 Hz, 1H), 4.51 (m, 2H), 4.33 (m, 2H), 4.02 (d, J=17.4 Hz, 1H), 3.94 (s, 3H), 2.96 (m, 1H), 1.30 (d, J=6.9 Hz, 6H), 0.77 (d, J=6.6 Hz, 3H). RTA IC50: 16 nM.

後処理

  1. customAfter further de-gassing with N2 and vacuum
  2. additionThe reaction was diluted with 50 mL ethyl acetate
  3. additionpoured into 100 mL
  4. washThe ethyl acetate layer was washed with brine (100 mL)
  5. filtrationfiltered through a 20 g plug of sodium sulfate
  6. washeluting with 50 mL ethyl acetate
  7. concentrationThe filtrate was concentrated
  8. customto purification with an X-Bridge 21.2×150 mm RP column
  9. washThe product of interest eluted in 80% portion of above gradient
  10. concentrationPure fractions (rich cut; impure discarded) were concentrated
  11. customto give product as a white solid

出典と根拠

ORDレコード
ord-783ea51cfd134d90bf43bda4de3104df
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353101B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート