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

HRID 2224747
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HRID 2224747 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e4186d779b8f4d9481f84cdcfb23036d
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07378447B2

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