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Benzyl Alcohol → 5-(Benzyloxy)-2-[4-(methanesulfonyl)piperazin-1-yl]pyrimidine

HRID 1723802
ノート
印刷プレビュー

反応式

HRID 1723802 の反応式
I[C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([S:14]([CH3:17])(=[O:16])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1.[CH2:18]([OH:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.N1C2C(=CC=C3C=2N=CC=C3)C=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>[Cu]I.C(Cl)Cl>[CH2:18]([O:25][C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([S:14]([CH3:17])(=[O:16])=[O:15])[CH2:10][CH2:9]2)=[N:6][CH:7]=1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=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 244Benzyl AlcoholHCID 13181,10-PhenanthrolineHCID 10796Cesium carbonateHCID 68849595HCID 68849595、化合物

生成物 1

HCID 688494605-(Benzyloxy)-2-[4-(methanesulfonyl)piperazin-1-yl]pyrimidine

試薬・触媒・溶媒 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 6344Dichloromethane溶媒

反応条件

温度
110 °C

実験手順

To a stirred suspension of 5-iodo-2-[4-(methylsulfonyl)piperazin-1-yl]pyrimidine (25.0 g, 67.9 mmol), benzyl alcohol (125 mL), 1,10-phenanthroline (2.45 g, 20 mol %), and cesium carbonate was added copper (I) iodide (12.9 g, 67.9 mmol) and the reaction heated to 110° C. for 90 minutes then cooled to room temperature. DCM (250 mL) was then added and the insolubles filtered off through a pad of celite. The cake washed with DCM (250 mL) and the DCM filtrates washed with water. The aqueous phase was then back extracted with more DCM (500 mL), the combined DCM extracts washed with brine (500 mL), dried (MgSO4), filtered and concentrated in vacuo to a dark brown sludge. This was then purified by flash chromatography (silica gel, 50% EtOAc/hexanes) to give 5-(benzyloxy)-2-[4-(methylsulfonyl)piperazin-1-yl]pyrimidine as an off white solid (14.2 g, 40.7 mmol, 60%).

後処理

  1. temperaturethen cooled to room temperature
  2. filtrationthe insolubles filtered off through a pad of celite
  3. washThe cake washed with DCM (250 mL)
  4. washthe DCM filtrates washed with water
  5. extractionThe aqueous phase was then back extracted with more DCM (500 mL)
  6. washthe combined DCM extracts washed with brine (500 mL)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo to a dark brown sludge
  10. customThis was then purified by flash chromatography (silica gel, 50% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-989f0aafda054a8da71621178447fa62
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07485644B2

反応ノート

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