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Triphenylarsine → (5R)-(-)-3-[4-(3-pyridyl)-3-fluorophenyl]-2-oxo-5-oxazolidinecarboxamide

HRID 1991240
ノート
印刷プレビュー

反応式

HRID 1991240 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][C@H:12]([C:14]([NH2:16])=[O:15])[O:11][C:10]2=[O:17])[CH:5]=[CH:6][C:7]=1I.C[Sn](C)(C)[C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.C1([As](C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>CN1CCCC1=O.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].[Cu]I>[N:22]1[CH:23]=[CH:24][CH:25]=[C:20]([C:7]2[CH:6]=[CH:5][C:4]([N:9]3[CH2:13][C@H:12]([C:14]([NH2:16])=[O:15])[O:11][C:10]3=[O:17])=[CH:3][C:2]=2[F:1])[CH:21]=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

8

反応物 3

HCID 11773Triphenylarsine2 回HCID 108684453-(Trimethylstannyl)pyridineHCID 68487894(5R)-(-)-3-[3-fluoro-4-iodophenyl]-2-oxo-5-oxazolidinecarboxamide

生成物 1

HCID 10214934(5R)-(-)-3-[4-(3-pyridyl)-3-fluorophenyl]-2-oxo-5-oxazolidinecarboxamide

試薬・触媒・溶媒 4

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
2 回
HCID 9811564Bis(dibenzylideneacetone)palladium触媒2 回
HCID 962Water溶媒
HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
50 °C

実験手順

A mixture of (5R)-(−)-3-[3-fluoro-4-iodophenyl]-2-oxo-5-oxazolidinecarboxamide (Step 3, 422 mg, 1.21 mmol), 3-(trimethylstannyl)pyridine (Step 4, 350 mg, 1.45 mmol), tris(dibenzylideneacetone)dipalladium(0) (22 mg, 0.0242 mmol), triphenylarsine (59 mg, 0.194 mmol) and copper(I) iodide (9 mg, 0.0484 mmol) in N-methyl-2-pyrrolidinone (4.8 mL) under nitrogen is degassed, heated up to 50° C. and stirred at this temperature for 2 days, during which additional tris(dibenzylideneacetone)dipalladium(0) (22 mg, 0.0242 mmol), triphenylarsine (59 mg, 0.194 mmol) and copper(I) iodide (9 mg, 0.0484 mmol) are added. The resulting mixture is diluted with water (15 mL) and extracted with methylene chloride (3×20 mL), and the combined organic phase is dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting oil is diluted with ethyl acetate (25 mL) and extracted with aqueous hydrochloric acid (1M, 25 mL), and the aqueous phase is neutralized with sodium hydroxide (s), saturated with sodium chloride and extracted with methylene chloride (3×25 mL) containing a small amount of methanol. This combined organic phase is dried over anhydrous sodium sulfate and concentrated under reduced pressure, and the residue is recrystallized from ethyl acetate/hexane to give the title compound, mp 240-242° C. (dec.); MS (ESI+) for C15H12FN3O3 m/z 302 (M+H)+; [α]25D=−25 (c 0.94, DMSO).

後処理

  1. customis degassed
  2. additionare added
  3. extractionextracted with methylene chloride (3×20 mL)
  4. dry with materialthe combined organic phase is dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionThe resulting oil is diluted with ethyl acetate (25 mL)
  7. extractionextracted with aqueous hydrochloric acid (1M, 25 mL)
  8. extractionextracted with methylene chloride (3×25 mL)
  9. additioncontaining a small amount of methanol
  10. dry with materialThis combined organic phase is dried over anhydrous sodium sulfate
  11. concentrationconcentrated under reduced pressure
  12. customthe residue is recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-0f3d91f7cb09434a926aa7b3cba7b605
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07645781B2

反応ノート

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