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2-(Pyridin-2-ylthio)ethanamine → N-(2-(pyridin-2-ylsulfanyl)ethyl)thioacetamide

HRID 2224747
ノート
印刷プレビュー

反応式

HRID 2224747 の反応式
[C:1]([N:4]1[C:12](=O)[C:11]2[C:6](=[CH:7]C=CC=2)C1=O)(=[S:3])C.[N:15]1[CH:20]=[CH:19]C=[CH:17][C:16]=1[S:21]CCN>C(Cl)(Cl)Cl>[N:4]1[CH:12]=[CH:11][CH:6]=[CH:7][C:1]=1[S:3][CH2:19][CH2:20][NH:15][C:16](=[S:21])[CH3:17]
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 2

HCID 40807472-(Pyridin-2-ylthio)ethanamineHCID 451186352-Ethanethioylisoindoline-1,3-dione

生成物 1

HCID 86607043N-(2-(pyridin-2-ylsulfanyl)ethyl)thioacetamide収率 58.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a mixture of 2-aminoethanethiol hydrochloride (4.07 g, 35.6 mmol) in dioxane (75 mL) at 50° C., add sodium hydride (60% in mineral oil, 2.84 g, 71.0 mmol) at room temperature under nitrogen. Allow the reaction to stir for 5 minutes and add 2-chloropyridine (3.5 mL, 37 mmol) to the mixture. Reflux the mixture for 24 hours and cool to room temperature. Add water (100 mL), and methylene chloride (300 mL) to this mixture. Extract the aqueous layer with methylene chloride (3×50 mL). Wash the combined organic phase with brine (200 mL), dry over magnesium sulfate, filter and concentrate to an orange oil. Flash chromatography on silica gel eluting with 50% (80:18:12 CHCl3/MeOH/concentrated NH4OH)/methylene chloride affords the title compound as a yellow oil (1.67 g, 30%). 1H NMR (CDCl3) δ 8.43 (m, 1H), 7.44 (m, 1H), 7.21 (m, 1H), 6.97 (m, 1H), 3.30 (m, 2H), 3.02 (m, 2H); MS (ES) m/z:═155 [C7H10N2S+H]+. Add 2-thioacetyl-isoindole-1,3-dione (0.7 g, 3.2 mmol) to a solution of 2-(pyridin-2-ylsulfanyl)ethylamine (0.5 g, 3.2 mmol) in CHCl3 (20 mL) at 0° C. After 15 minutes, concentrate and purify the residue by flash chromatography on silica gel eluting with 40% EtOAc/Hex containing 2% NH4OH to afford N-(2-(pyridin-2-ylsulfanyl)ethyl)thioacetamide (0.4 g, 58%) as a pale yellow oil. 1H NMR (CDCl3) δ 10.26 (br s, 1H), 8.41-8.43 (m, 1H), 7.57 (dt, J=7.35 Hz, J=1.8 Hz, 1H), 7.31 (dd, J=8.10 Hz, J=0.96 Hz, 1H), 7.09-7.13 (m, 1H), 3.87-3.92 (m, 2H), 3.40-3.43 (m, 2H), 2.53 (s, 3H); MS (APCI): m/z 213 (M+H).

後処理

  1. customat 0° C
  2. concentrationconcentrate
  3. custompurify the residue by flash chromatography on silica gel eluting with 40% EtOAc/Hex
  4. additioncontaining 2% NH4OH

出典と根拠

ORDレコード
ord-e4186d779b8f4d9481f84cdcfb23036d
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07378447B2

反応ノート

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