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Cesium carbonate → 3-(5-Bromopyridin-3-yl)oxazolidin-2-one

HRID 712761
ノート
印刷プレビュー

反応式

HRID 712761 の反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6](I)[CH:7]=1.[O:9]1[CH2:13][C:12](=O)[N:11]=[C-:10]1.C1(P(C2C=CC=CC=2)C2C3[O:34]C4C(=CC=CC=4P(C4C=CC=CC=4)C4C=CC=CC=4)C(C)(C)C=3C=CC=2)C=CC=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>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].C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[C:6]([N:11]2[CH2:12][CH2:13][O:9][C:10]2=[O:34])[CH:5]=[N:4][CH:3]=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 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 8204093-Bromo-5-iodopyridineHCID 532495662H-1,3-oxazol-2-id-4-one

生成物 1

HCID 679825123-(5-Bromopyridin-3-yl)oxazolidin-2-one収率 232.9%

試薬・触媒・溶媒 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

An argon purged flask (100 mL) is charged with reagent 3-bromo-5-iodopyridine (200 mg, 0.704 mmol), 2-oxazolidone (61.3 mg, 0.704 mmol), tris(dibenzylideneacetone)dipalladium(0) (64.5 mg, 0.07 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (61.1 mg, 0.106 mmol), and cesium carbonate (459 mg, 1.409 mmol). Toluene (bubbled with argon before use, 14 mL) is then added. The resulting mixture is heated at 90° C. under argon for 16 h. The mixture is filtered through diatomaceous earth and washed with MeOH (30 mL). The filtrate is concentrated. The resulting crude product is purified by normal phase chromatography using 0-4.5% MeOH in DCM as the gradient to afford 3-(5-bromo-pyridin-3-yl)-oxazolidin-2-one (60 mg, 35% yield).

後処理

  1. filtrationThe mixture is filtered through diatomaceous earth
  2. washwashed with MeOH (30 mL)
  3. concentrationThe filtrate is concentrated
  4. customThe resulting crude product is purified by normal phase chromatography

出典と根拠

ORDレコード
ord-a74c260997024399b59abd22c9e732e5
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181272B2

反応ノート

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