Cesium carbonate → HCID 86617330, 화합물

HRID 1918451노트

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HRID 1918451 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 86617330HCID 86617330, 화합물수율 75%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-38c81e392ca843b1ba537ae6ca9d58a5
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618329B2

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