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Cesium carbonate → HCID 86720999、化合物

HRID 524941
ノート
印刷プレビュー

反応式

HRID 524941 の反応式
CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.I[C:44]1[C:45]([O:59][CH3:60])=[CH:46][C:47]([N:50]([CH3:58])[C:51](=[O:57])[O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[N:48][CH:49]=1.[C:61]1([C:67]([C:69]2[CH:74]=[CH:73][CH:72]=[CH:71][CH:70]=2)=[NH:68])[CH:66]=[CH:65][CH:64]=[CH:63][CH:62]=1.C([O-])([O-])=O.[Cs+].[Cs+]>O1CCOCC1.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]>[C:61]1([C:67](=[N:68][C:44]2[C:45]([O:59][CH3:60])=[CH:46][C:47]([N:50]([CH3:58])[C:51](=[O:57])[O:52][C:53]([CH3:56])([CH3:55])[CH3:54])=[N:48][CH:49]=2)[C:69]2[CH:70]=[CH:71][CH:72]=[CH:73][CH:74]=2)[CH:66]=[CH:65][CH:64]=[CH:63][CH:62]=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 136809Benzophenone imineHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 58053580HCID 58053580、化合物

生成物 1

HCID 86720999HCID 86720999、化合物収率 69.3%

試薬・触媒・溶媒 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

Pd2(dba)3 (33.70 mg, 0.03680 mmol) and Xantphos (42.58 mg, 0.07359 mmol) were added to a sealed tube containing tert-butyl N-(5-iodo-4-methoxy-2-pyridyl)-N-methyl-carbamate (268 mg, 0.7359 mmol), diphenylmethanimine (173.4 mg, 160.6 μL, 0.9567 mmol) and Cs2CO3 (719.4 mg, 2.208 mmol) in dioxane (2.5 mL). The reaction was placed under an atmosphere of nitrogen and heated at 100° C. for 4 hours. At RT, the reaction mixture was filtered through celite and the filtrate concentrated in vacuo. The residue was purified by column chromatography (ISCO Companion, 40 g column, eluting with 0 to 30% EtOAc/Petroleum Ether, loaded in DCM) to give tert-butyl (5-((diphenylmethylene)amino)-4-methoxypyridin-2-yl)(methyl)carbamate as a yellow solid (213 mg, 69% Yield). MS (ES+) 418.2.

後処理

  1. filtrationAt RT, the reaction mixture was filtered through celite
  2. concentrationthe filtrate concentrated in vacuo
  3. customThe residue was purified by column chromatography (ISCO Companion, 40 g column, eluting with 0 to 30% EtOAc/Petroleum Ether, loaded in DCM)

出典と根拠

ORDレコード
ord-850e54f3b4204319adf7693692a72315
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09340546B2

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