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Potassium Phosphate, Tribasic → (2-(4-Chloro-phenyl)-2-[4-(1H-pyrazol-4-yl)-phenyl]-ethyl)-methyl-amine

HRID 1798366
ノート
印刷プレビュー

反応式

HRID 1798366 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)[CH2:9][NH:10][CH3:11])=[CH:4][CH:3]=1.CC1(C)C(C)(C)OB([C:27]2[CH:28]=[N:29][NH:30][CH:31]=2)O1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>C(O)C.CO.C1(C)C=CC=CC=1.O.CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[Cl:18][C:15]1[CH:16]=[CH:17][C:12]([CH:8]([C:5]2[CH:6]=[CH:7][C:2]([C:27]3[CH:28]=[N:29][NH:30][CH:31]=3)=[CH:3][CH:4]=2)[CH2:9][NH:10][CH3:11])=[CH:13][CH:14]=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

9

反応物 3

HCID 62657Potassium Phosphate, TribasicHCID 27740104-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazoleHCID 57691393[2-(4-Bromo-phenyl)-2-(4-chloro-phenyl)ethyl]-methyl-amine

生成物 1

HCID 11438353(2-(4-Chloro-phenyl)-2-[4-(1H-pyrazol-4-yl)-phenyl]-ethyl)-methyl-amine収率 84.2%

試薬・触媒・溶媒 5

HCID 178418851
HCID 178418851、化合物
触媒
HCID 702Ethanol溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

反応条件

温度
80 °C

実験手順

A solution of [2-(4-Bromo-phenyl)-2-(4-chloro-phenyl)-ethyl]-methyl-amine (6.1 g, 13.716 mmol), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (5.3 g, 27.431 mmol) and K3PO4 (10.19 g, 48.00 mmol) in ethanol (7.5 ml), methanol (11.5 ml), toluene (7.5 ml) and water (11.5 ml) was purged with nitrogen for 2 minutes. Bis(tri-t-butylphosphine)palladium (0) (175 mg, 2.5 mol %) was then added and the reaction mixture purged with nitrogen for a further 2 minutes. The mixture was then heated to 80° C., under nitrogen for a period of 17 hours. The solvents were removed and the residue was partitioned between ethyl acetate and 2N NaOH. The aqueous layer was extracted with ethyl acetate and the combined organic layers were washed with brine, dried (MgSO4) and concentrated under reduced pressure. The crude reaction mixture was purified by column chromatography (SiO2), eluting with dichloromethane: methanol: acetic acid:water (90:18:3:2) to afford the title compound (3.6 g); LCMS (PS-A2) Rt 2.08 min [M+H]+ 312.

後処理

  1. customthe reaction mixture purged with nitrogen for a further 2 minutes
  2. customThe solvents were removed
  3. customthe residue was partitioned between ethyl acetate and 2N NaOH
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. washthe combined organic layers were washed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure
  8. customThe crude reaction mixture
  9. customwas purified by column chromatography (SiO2)
  10. washeluting with dichloromethane: methanol: acetic acid:water (90:18:3:2)

出典と根拠

ORDレコード
ord-b0a726fbb4cd422db7f33c27beaccbf9
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08343953B2

反応ノート

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