Cesium carbonate → HCID 86617330、化合物

HRID 1960211ノート

反応式

HRID 1960211 の反応式
I[C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:10]=[CH:11][O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[C:32](P(C(C)(C)C)C(C)(C)C)(C)(C)[CH3:33].C([Sn](CCCC)(CCCC)C=C)CCC>O1CCOCC1>[CH:32]([C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]([O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:10]=[CH:11][O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1)=[CH2:33]

参加物

6

反応物 4

HCID 10796Cesium carbonateHCID 81998TributylvinyltinHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 86617331HCID 86617331、化合物

生成物 1

HCID 86617330HCID 86617330、化合物収率 75%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

Phenyl N-(4-iodophenyl)-3-(phenoxy)acrylimidate (0.50 g), bis(benzylideneacetone)palladium (0) (0.023 g) and cesium carbonate (0.82 g) were suspended to dioxane (15 ml). Tri-t-butylphosphine (10 wt % in hexane: 0.24 g) and tributyl (vinyl) tin (0.44 g) were added thereto and it was stirred for four hours at room temperature and 60° C. for five hours. The unsolved matter was filtered off, and the filtrate was concentrated under reduced pressure. The residue was separated and purified by silica gel column chromatography (hexane:ethyl acetate=30:1) to obtain phenyl N-(4-vinylphenyl)-3-(phenoxy)acrylimidate (0.29 g) as yellow oil.

後処理

  1. filtrationThe unsolved matter was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was separated
  4. custompurified by silica gel column chromatography (hexane:ethyl acetate=30:1)

出典と根拠

ORDレコード
ord-4f4b74eb225c406a80bdc46e7110eba4
出典データセット
uspto-grants-2013_04
特許番号
US08410316B2

反応ノート

読み込み中…