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Methional → HCID 53672169、化合物

HRID 581646
ノート
印刷プレビュー

反応式

HRID 581646 の反応式
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]
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

7

反応物 4

HCID 18635MethionalHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 126902953-Chloropropylmethylsulfane

生成物 1

HCID 53672169HCID 53672169、化合物収率 36%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e4470f0358c64569bf7586efdb5fb652
出典データセット
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05922527

反応ノート

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