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Iodoethane → HCID 15745497、化合物

HRID 2051589
ノート
印刷プレビュー

反応式

HRID 2051589 の反応式
[NH2:1][C@H:2]([CH2:7][OH:8])[CH2:3][CH:4]([CH3:6])[CH3:5].[H-].[Na+].[CH2:11](I)[CH3:12]>C1COCC1>[CH2:11]([O:8][CH2:7][C@@H:2]([NH2:1])[CH2:3][CH:4]([CH3:6])[CH3:5])[CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6340IodoethaneHCID 24758Sodium hydride2 回HCID 111307L-Leucinol

生成物 1

HCID 15745497HCID 15745497、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

(S)-leucinol (6.4 mL, 5 mmol) was added over 30 minutes to a well stirred slurry of 6% sodium hydride (2.2 g, 55 mmol) in THF (50 mL) at room temperature under N2. After all of the sodium hydride had reacted, a solution of ethyl iodide (4 mL, 50 mmol) in THF (50 mL) was added and the reaction stirred at 20°-25° C. for 20 hours. THF was removed under reduced pressure and the residue partitioned between diethyl ether and brine. The ether extract was dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was flash chromatographed over silica gel and pure aminoether eluted with a mixture of 10% isopropanol and 90% chloroform.

後処理

  1. customTHF was removed under reduced pressure
  2. customthe residue partitioned between diethyl ether and brine
  3. extractionThe ether extract
  4. dry with materialwas dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customchromatographed over silica gel and pure aminoether
  8. washeluted with a mixture of 10% isopropanol and 90% chloroform

出典と根拠

ORDレコード
ord-a3f3f228b85f44478248a16dd029eeff
出典データセット
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05019647

反応ノート

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