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Ethyl Acetate → HCID 22000062、化合物

HRID 1975948
ノート
印刷プレビュー

反応式

HRID 1975948 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][C:4]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[CH3:15].C[Si](C)(C)[N-][Si](C)(C)C.[K+].[F:26][C:27]([F:45])([F:44])[C:28]1[CH:29]=[C:30]([C:38]([CH3:43])([CH3:42])[C:39](Cl)=[O:40])[CH:31]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:33]=1.C(OCC)(=O)C>CN(C)C=O.O1CCCC1>[F:26][C:27]([F:45])([F:44])[C:28]1[CH:29]=[C:30]([C:38]([CH3:43])([CH3:42])[C:39]([N:2]([CH3:1])[C:3]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH3:15])=[O:40])[CH:31]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:33]=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 8857Ethyl AcetateHCID 3251421Potassium bis(trimethylsilyl)amideHCID 112671412-(3,5-Bis(trifluoromethyl)phenyl)-2-methylpropanoyl chlorideHCID 22000072HCID 22000072、化合物

生成物 1

HCID 22000062HCID 22000062、化合物収率 61.9%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of 140 mg (0.71 mmol) methyl-(3-o-tolyl-pyridin-4-yl)-amine in 1 ml N,N-dimethylformamide at 0° C. were added dropwise 0.71 ml (0.71 mmol) of 1 M potassium hexamethyldisilazide solution in tetrahydrofuran. Stirring was continued for 1 h at room temperature and the reaction mixture was cooled to 0° C. again. At this temperature, a solution of 270 mg (0.85 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride in 0.5 ml tetrahydrofuran was added. After stirring for 18 h at room temperature, ethyl acetate was added and the organic phase was washed with brine, dried (magnesium sulfate) and evaporated. The residue was purified by flash chromatography to give 211 mg (58%) of the title compound as white foam.

後処理

  1. stirringAfter stirring for 18 h at room temperature
  2. washthe organic phase was washed with brine
  3. dry with materialdried (magnesium sulfate)
  4. customevaporated
  5. customThe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-8c28b74508b24bbe87e9a45654736211
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06225316B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート