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Methional → HCID 53672169, 화합물

HRID 581646
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HRID 581646 반응식
Cl[CH2:2][CH2:3][CH2:4][S:5][CH3:6].[Mg].[CH3:8][S:9][CH2:10][CH2:11][CH:12]=[O:13].[Cl-].[NH4+]>C1COCC1.CCOCC>[CH3:8][S:9][CH2:10][CH2:11][CH:12]([OH:13])[CH2:2][CH2:3][CH2:4][S:5][CH3:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 18635MethionalHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 126902953-Chloropropylmethylsulfane

생성물 1

HCID 53672169HCID 53672169, 화합물수율 36%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

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온도
50 °C

실험 절차

1-Chloro-3-methylthiopropane (3.73 g, 30 mmole) in dry THF (50 mL) was added to stirred magnesium turnings (0.72 g, 30 mmole) under argon. Once the addition was complete, the mixture was heated to 50° C. for 3 hours. The mixture was then allowed to cool to room temperature and 3-methylthiopropanal (3.12 g, 30 mmole) was added. The reaction was stirred at room temperature for 1 hour. 2M ammonium chloride solution (50 mL) was added, followed by ether (50 mL). The organics were separated, dried, filtered, and evaporated to give a pale yellow oil that was purified by chromatography in 40-60 petroleum ether/ether (4/5) to give 5 (2.1 g, 36%) as a colorless oil.

후처리

  1. additionOnce the addition
  2. temperatureto cool to room temperature
  3. customThe organics were separated
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customto give a pale yellow oil that
  8. customwas purified by chromatography in 40-60 petroleum ether/ether (4/5)

출처 및 근거

ORD 기록
ord-e4470f0358c64569bf7586efdb5fb652
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05922527

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