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Toluene → 2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(1 (S),2-dihydroxy-2-methyl-propyl)-pyrazin-2-yl]-propionamide

HRID 719977
ノート
印刷プレビュー

反応式

HRID 719977 の反応式
[C:1](=[O:4])([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:9]=[C:10]([C@@H:18]([CH2:32][CH:33]2[CH2:37][CH2:36][CH2:35][CH2:34]2)[C:19]([NH:21][C:22]2[CH:27]=[N:26][C:25](C=C(C)C)=[CH:24][N:23]=2)=[O:20])[CH:11]=[CH:12][C:13]=1[S:14]([CH3:17])(=[O:16])=[O:15].CS(N)(=O)=O.S([O-])([O-])=[O:44].[Na+].[Na+].[C:49]1([CH3:55])C=CC=C[CH:50]=1>C(OCC)(=O)C.[Fe-3](C#N)(C#N)(C#N)(C#N)(C#N)C#N.[K+].[K+].[K+].[Os](=O)(=O)(=O)=O.CC[C@H]1[C@H]2C[C@H]([C@H](OC3C4C(=CC=CC=4)C(O[C@H](C4C=CN=C5C=4C=C(OC)C=C5)[C@@H]4N5C[C@H](CC)[C@@H](CC5)C4)=NN=3)C3C=CN=C4C=3C=C(OC)C=C4)N(CC2)C1.O.C(O)(C)(C)C>[Cl:7][C:8]1[CH:9]=[C:10]([C@@H:18]([CH2:32][CH:33]2[CH2:34][CH2:35][CH2:36][CH2:37]2)[C:19]([NH:21][C:22]2[CH:27]=[N:26][C:25]([C@H:1]([OH:4])[C:49]([OH:44])([CH3:55])[CH3:50])=[CH:24][N:23]=2)=[O:20])[CH:11]=[CH:12][C:13]=1[S:14]([CH3:17])(=[O:16])=[O:15]
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

11

反応物 5

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 24437Sodium SulfiteHCID 72879MethanesulfonamideHCID 674827762(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(2-methylpropenyl)-pyrazin-2-yl]-propionamide

生成物 1

HCID 10413475
2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(1 (S),2-dihydroxy-2-methyl-propyl)-pyrazin-2-yl]-propionamide
収率 69%

試薬・触媒・溶媒 5

HCID 30318Osmium Tetroxide触媒HCID 510036741-((1R)-((2R,4R,5S)-5-ethylquinuclidin-2-yl)(6-methoxyquinolin-4-yl)methoxy)-4-((1R)-((2R,4S,5R)-5-ethylquinuclidin-2-yl)(6-methoxyquinolin-4-yl)methoxy)phthalazine触媒HCID 178511488HCID 178511488、化合物触媒HCID 8857Ethyl Acetate溶媒HCID 714019492-Methylpropan-2-ol--water (1/1)溶媒

反応条件

温度
25 °C

実験手順

A mixture of potassium ferricyanide (738 mg, 2.24 mmol), potassium carbonate (310 mg, 2.24 mmol), and (DHQ)2PHAL (11.7 mg, 0.015 mmol) was treated with a solution of water/tert-butyl alcohol (15 mL, 1:1) and stirred at 25° C. to give a clear solution. The reaction mixture was then treated with a 0.2M solution of osmium tetroxide in toluene (37.4 μL). The reaction mixture was cooled to 0° C. and then was treated with 2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(2-methylpropenyl)-pyrazin-2-yl]-propionamide (345 mg, 0.748 mmol) followed by the addition of methane sulfonamide (71 mg, 0.747 mmol). The mixture was stirred at 0° C. for 18 h until all the olefin was reacted. The mixture was diluted with ethyl acetate (30 mL) and treated with sodium sulfite (1.0 g). The solution was extracted with ethyl acetate and water. The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230–400 mesh, 1/5 hexanes/ethyl acetate) afforded 2(R)-(3-chloro-4-methanesulfonyl-phenyl)-3-cyclopentyl-N-[5-(1(S),2-dihydroxy-2-methyl-propyl)-pyrazin-2-yl]-propionamide (255 mg, 69%) as an off-white foam: (ES)+-HRMS m/e calcd for C23H30ClN3O5S (M+H)+ 496.1668, found 496.1657.

後処理

  1. customto give a clear solution
  2. temperatureThe reaction mixture was cooled to 0° C.
  3. customwas reacted
  4. extractionThe solution was extracted with ethyl acetate and water
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2b157337404347a6b4bb43115230e3fb
出典データセット
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07132425B2

反応ノート

読み込み中…

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