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Potassium Carbonate → 3-(3-Ethynylphenyl)-2-(2,4,6-trifluorobenzyl)-7-(trifluoromethyl)-2H-indazole

HRID 735449
ノート
印刷プレビュー

反応式

HRID 735449 の反応式
[F:1][C:2]1[CH:33]=[C:32]([F:34])[CH:31]=[C:30]([F:35])[C:3]=1[CH2:4][N:5]1[C:13]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]#[C:21][Si](C)(C)C)[CH:15]=2)=[C:12]2[C:7]([C:8]([C:26]([F:29])([F:28])[F:27])=[CH:9][CH:10]=[CH:11]2)=[N:6]1.C(=O)([O-])[O-].[K+].[K+]>CO>[C:20]([C:16]1[CH:15]=[C:14]([C:13]2[N:5]([CH2:4][C:3]3[C:30]([F:35])=[CH:31][C:32]([F:34])=[CH:33][C:2]=3[F:1])[N:6]=[C:7]3[C:12]=2[CH:11]=[CH:10][CH:9]=[C:8]3[C:26]([F:29])([F:27])[F:28])[CH:19]=[CH:18][CH:17]=1)#[CH:21]
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

4

反応物 2

HCID 11430Potassium CarbonateHCID 866030102-(2,4,6-Trifluorobenzyl)-7-(trifluoromethyl)-3-{3-[(trimethylsilyl)ethynyl]phenyl}-2H-indazole

生成物 1

HCID 866030133-(3-Ethynylphenyl)-2-(2,4,6-trifluorobenzyl)-7-(trifluoromethyl)-2H-indazole収率 91.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

A mixture of 2-(2,4,6-trifluorobenzyl)-7-(trifluoromethyl)-3-{3-[(trimethylsilyl)-ethynyl]phenyl}-2H-indazole (1.78 g, 3.54 mmol) and potassium carbonate (0.49 g, 3.54 mmol) in 50 mL of methanol was heated at 50° C. for 2 hours. The reaction mixture was concentrated in vacuo and the residue partitioned between ethyl acetate and H2O. The organic phase was dried (Na2SO4) and concentrated in vacuo to give 1.4 g of a white solid, which was purified by flash chromatography (silica gel 60, hexane-ethyl acetate, 4:1) to give 1.1 g of the title compound.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue partitioned between ethyl acetate and H2O
  3. dry with materialThe organic phase was dried (Na2SO4)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f6c3b4208cae47368f783b6806385578
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592363B2

反応ノート

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