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Cesium carbonate → Tert-butyl (4-((2-methyl-6-nitropyridin-3-yl)oxy)pyridin-2-yl)carbamate

HRID 626569
ノート
印刷プレビュー

反応式

HRID 626569 の反応式
Cl[C:2]1[CH:7]=[C:6]([O:8][C:9]2[C:10]([CH3:18])=[N:11][C:12]([N+:15]([O-:17])=[O:16])=[CH:13][CH:14]=2)[CH:5]=[CH:4][N:3]=1.[C:19](=[O:26])([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[NH2:20].C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.[Fe+2].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]>[CH3:18][C:10]1[C:9]([O:8][C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH:20][C:19](=[O:26])[O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[CH:7]=2)=[CH:14][CH:13]=[C:12]([N+:15]([O-:17])=[O:16])[N:11]=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 3

HCID 10796Cesium carbonateHCID 77922tert-Butyl carbamateHCID 904036213-((2-Chloropyridin-4-yl)oxy)-2-methyl-6-nitropyridine

生成物 1

HCID 131735225Tert-butyl (4-((2-methyl-6-nitropyridin-3-yl)oxy)pyridin-2-yl)carbamate収率 29.1%

試薬・触媒・溶媒 3

HCID 635956Ferrocene-1,1'-bis-(diphenylphosphine)
触媒
HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A mixture of Example A3 (1.2 g, 4.52 mmol), t-butyl carbamate (1.058 g, 9.03 mmol), Cs2CO3 (2.94 g, 9.03 mmol) and DPPF (0.351 g, 0.632 mmol) in dioxane (25 mL) was sparged with Ar, treated with Pd2(dba)3 (0.290 g, 0.316 mmol), sparged again with Ar and heated at 100° C. for 3 days. The mixture was cooled to RT, diluted with EtOAc, the solids removed via filtration through diatomaceous earth and the filtrate concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford tert-butyl (4-((2-methyl-6-nitropyridin-3-yl)oxy)pyridin-2-yl)carbamate (456 mg, 29%). MS (ESI) m/z: 347.2 (M+H+).

後処理

  1. customsparged again with Ar
  2. temperatureThe mixture was cooled to RT
  3. additiondiluted with EtOAc
  4. customthe solids removed via filtration through diatomaceous earth
  5. concentrationthe filtrate concentrated to dryness
  6. custompurified via silica gel chromatography (EtOAc/Hex)

出典と根拠

ORDレコード
ord-383f2caff4064bbbb9f6c7fb2fb266c8
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09309224B2

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