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Potassium Carbonate → HCID 68828548、化合物

HRID 1727369
ノート
印刷プレビュー

反応式

HRID 1727369 の反応式
[Cl:1][CH2:2][C:3]1[CH:8]=[C:7]([C:9]2[S:13][C:12]([CH2:14][CH3:15])=[N:11][C:10]=2[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=2)[CH:6]=[CH:5][N:4]=1.C(=O)([O-])[O-].[K+].[K+].[NH:29]1[CH2:33][CH2:32][CH2:31][CH2:30]1>>[ClH:1].[ClH:1].[CH2:14]([C:12]1[S:13][C:9]([C:7]2[CH:6]=[CH:5][N:4]=[C:3]([CH2:2][N:29]3[CH2:33][CH2:32][CH2:31][CH2:30]3)[CH:8]=2)=[C:10]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([CH3:22])[CH:17]=2)[N:11]=1)[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 229326995-(2-Chloromethyl-4-pyridyl)-2-ethyl-4-(3-methylphenyl)-1,3-thiazole

生成物 1

HCID 68828548HCID 68828548、化合物収率 85%

実験手順

To a solution of 5-(2-chloromethyl-4-pyridyl)-2-ethyl-4-(3-methylphenyl)-1,3-thiazole (0.20 g, 0.61 mmol) in pyrrolidine (0.5 mL) was stirred for 1 hour at 80° C. After cooling, to this was added an aqueous potassium carbonate solution, and extracted with ethyl acetate. The extracts were washed with brine, then, dried and concentrated. The residue was purified by alumina column chromatography (hexane-ethyl acetate=2:1). The resulting oil was made into a hydrochloride by using a solution of 4N-hydrogen chloride in ethyl acetate, and recrystallized from ethanol-isopropyl ether, to obtain a title compound (0.23 g, 85%).

後処理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe extracts were washed with brine
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by alumina column chromatography (hexane-ethyl acetate=2:1)
  7. customrecrystallized from ethanol-isopropyl ether

出典と根拠

ORDレコード
ord-5980c7a72ace49bd9ea4021d83b2004e
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07495018B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート