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Dichloromethane → HCID 178424071、化合物

HRID 1353753
ノート
印刷プレビュー

反応式

HRID 1353753 の反応式
Br[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[N:15]=[CH:14][N:13](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:12]=3)[CH:9]=2)[N:4](C2CCCCO2)[N:3]=1.[CH3:41][C:42]1[CH:47]=[CH:46][C:45](B(O)O)=[CH:44][CH:43]=1.ClCCl.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>COCCOC.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[CH3:41][C:42]1[CH:47]=[CH:46][C:45]([C:2]2[C:10]3[C:5](=[CH:6][CH:7]=[C:8]([C:11]4[N:15]=[CH:14][NH:13][N:12]=4)[CH:9]=3)[NH:4][N:3]=2)=[CH:44][CH:43]=1
参加物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 6344DichloromethaneHCID 62657Potassium Phosphate, TribasicHCID 79799Tolylboronic acidHCID 22479811HCID 22479811、化合物

生成物 1

HCID 178424071HCID 178424071、化合物収率 185.9%

試薬・触媒・溶媒 2

HCID 635956
Ferrocene-1,1'-bis-(diphenylphosphine)
触媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of 2-{3-bromo-5-[1-(triphenylmethyl)(1,2,4-triazol-3-yl)]-1H-indazolyl}perhydro-2H-pyran (0.150 g, 0.254 mmol), in ethylene glycol dimethyl ether (3 mL) was added 4-methylphenyl boronic acid (0.052 g, 0.381 mmol), [1,1′-bis(diphenylphosphino)-ferrocene] complex with dichloromethane (1:1) (0.030 g, 0.0254 mmol) and potassium phosphate (0.269 g, 1.27 mmol). The reaction mixture was heated to reflux temperature for 5 hours. The solvent was then evaporated to dryness and the residue was dissolved in 20 mL of ethyl acetate. The heterogeneous solution was washed 3 times with 10 mL of water and once with 10 mL of brine. The organic layer was dried over Na2SO4 and evaporated to dryness. The resulting brown solid was adsorbed on silica gel and purified by column chromatography (85:15 hexanes/ethyl acetate) to provide the title compound (0.130 g, 85% yield): ES-MS (m/z) 602 [M+1]+.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux temperature for 5 hours
  3. customThe solvent was then evaporated to dryness
  4. dissolutionthe residue was dissolved in 20 mL of ethyl acetate
  5. washThe heterogeneous solution was washed 3 times with 10 mL of water
  6. dry with materialThe organic layer was dried over Na2SO4
  7. customevaporated to dryness
  8. custompurified by column chromatography (85:15 hexanes/ethyl acetate)

出典と根拠

ORDレコード
ord-efad0ace1294457ea86ed781d138e75e
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220771B2

反応ノート

読み込み中…

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