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Cesium carbonate → Tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate

HRID 2406770
ノート
印刷プレビュー

反応式

HRID 2406770 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.[NH2:43][C:44]1[N:49]=[C:48]([NH:50][C@H:51]2[CH2:56][CH2:55][CH2:54][CH2:53][C@H:52]2[NH:57][C:58](=[O:64])[O:59][C:60]([CH3:63])([CH3:62])[CH3:61])[C:47]([Cl:65])=[CH:46][C:45]=1[C:66]([NH:68][C:69]([C:72]1[CH:77]=[CH:76][CH:75]=[CH:74][CH:73]=1)([CH3:71])[CH3:70])=[O:67].C(=O)([O-])[O-].[Cs+].[Cs+].Br[C:85]1[CH:86]=[N:87][CH:88]=[C:89]([CH3:91])[CH:90]=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(OCC)(=O)C.O.O1CCOCC1>[Cl:65][C:47]1[C:48]([NH:50][C@H:51]2[CH2:56][CH2:55][CH2:54][CH2:53][C@H:52]2[NH:57][C:58](=[O:64])[O:59][C:60]([CH3:63])([CH3:61])[CH3:62])=[N:49][C:44]([NH:43][C:85]2[CH:86]=[N:87][CH:88]=[C:89]([CH3:91])[CH:90]=2)=[C:45]([C:66]([NH:68][C:69]([C:72]2[CH:73]=[CH:74][CH:75]=[CH:76][CH:77]=2)([CH3:70])[CH3:71])=[O:67])[CH:46]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 8177133-Bromo-5-methylpyridineHCID 86683895Tert-butyl cis-2-(6-amino-3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate

生成物 1

HCID 86683894
Tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate
収率 55%

試薬・触媒・溶媒 4

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

Xantphos (5 mg) and Pd2(dba)3 (4 mg) were added to a mixture of tert-butyl cis-2-(6-amino-3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)pyridin-2-ylamino)cyclohexylcarbamate (20 mg), cesium carbonate (20 mg), 3-bromo-5-methylpyridine (9 mg), and 1,4-dioxane (2 ml) in a nitrogen atmosphere, followed by reflux for 3 hours in a nitrogen atmosphere. The reaction mixture was cooled to room temperature, and water and ethyl acetate were added. The organic layer was collected, washed with saturated saline, and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel chromatography (silica gel: Kanto Chemical Co., Inc., silica gel 60 (spherical shape), hexane•ethyl acetate=2:1 to 3:1), and a white solid of tert-butyl cis-2-(3-chloro-5-(2-phenylpropan-2-ylaminocarbonyl)-6-(5-methylpyridin-3-ylamino)pyridin-2-ylamino)cyclohexylcarbamate (13 mg) was thus obtained.

後処理

  1. temperatureby reflux for 3 hours in a nitrogen atmosphere
  2. customThe organic layer was collected
  3. washwashed with saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled away under reduced pressure
  6. customThe obtained residue was purified by silica gel chromatography (silica gel: Kanto Chemical Co., Inc., silica gel 60 (spherical shape), hexane•ethyl acetate=2:1 to 3:1)

出典と根拠

ORDレコード
ord-3df51c879d77472fbd329768eda0602d
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809371B2

反応ノート

読み込み中…

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