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Potassium tert-butoxide → HCID 178464054、化合物

HRID 1620476
ノート
印刷プレビュー

反応式

HRID 1620476 の反応式
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:15]=[CH:14][C:4]=1[CH2:5][N:6]1[CH2:11][CH2:10][CH:9]([CH:12]=O)[CH2:8][CH2:7]1.[CH2:24]([N:26]([CH2:36][CH3:37])[CH2:27][CH2:28][NH:29][C:30]1[CH2:34][S:33][C:32](=[O:35])[N:31]=1)[CH3:25].CC(C)([O-])C.[K+]>C(O)C>[F:23][C:2]([F:1])([F:22])[C:3]1[CH:17]=[C:16]([C:18]([F:20])([F:21])[F:19])[CH:15]=[CH:14][C:4]=1[CH2:5][N:6]1[CH2:7][CH2:8][CH:9](/[CH:12]=[C:34]2/[C:30]([NH:29][CH2:28][CH2:27][N:26]([CH2:36][CH3:37])[CH2:24][CH3:25])=[N:31][C:32](=[O:35])[S:33]/2)[CH2:10][CH2:11]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

5

反応物 3

HCID 23665647Potassium tert-butoxideHCID 866786631-[2,4-Bis(trifluoromethyl)benzyl]piperidine-4-carbaldehydeHCID 178464053HCID 178464053、化合物

生成物 1

HCID 178464054HCID 178464054、化合物収率 74.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To a solution of 1-[2,4-bis(trifluoromethyl)benzyl]piperidine-4-carbaldehyde (6.64 g) and 4-{[2-(diethylamino)ethyl]amino}-1,3-thiazol-2(5H)-one (5.48 g) in ethanol (98 mL) was added potassium tert-butoxide (2.85 g). The reaction mixture was stirred at 80° C. for 20 min, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane). The solvent was evaporated under reduced pressure, the residue was dissolved in ethyl acetate, the solution was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, methanol/ethyl acetate) and further silica gel column chromatography (methanol/ethyl acetate) to give the title compound (7.84 g).

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)
  3. customThe solvent was evaporated under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washthe solution was washed with water and saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (NH, methanol/ethyl acetate) and further silica gel column chromatography (methanol/ethyl acetate)

出典と根拠

ORDレコード
ord-4440e8c9393b456984e75e56298fcd66
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772277B2

反応ノート

読み込み中…

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