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Ethyl chloroacetate → (5S)-5-cyclopropylmorpholin-3-one

HRID 2366353
ノート
印刷プレビュー

反応式

HRID 2366353 の反応式
[H-].[Na+].[NH2:3][C@@H:4]([CH:7]1[CH2:9][CH2:8]1)[CH2:5][OH:6].Cl[CH2:11][C:12](OCC)=[O:13]>C1(C)C=CC=CC=1>[CH:7]1([C@@H:4]2[NH:3][C:12](=[O:13])[CH2:11][O:6][CH2:5]2)[CH2:9][CH2:8]1
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 7751Ethyl chloroacetateHCID 24758Sodium hydrideHCID 55283785(2S)-2-amino-2-cyclopropylethan-1-ol

生成物 1

HCID 58074457(5S)-5-cyclopropylmorpholin-3-one収率 21.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒3 回

実験手順

To a cold, stirred suspension of sodium hydride (600 mg, 14.99 mmol) in toluene (20 mL) was added dropwise a solution of (S)-2-amino-2-cyclopropylethanol (680 mg, 6.72 mmol)) in toluene (12 mL). The reaction mixture was then allowed to warm to room temperature and a solution of ethyl chloroacetate (824 mg, 6.72 mmol) in toluene (4 mL) was added dropwise. The resulting mixture was stirred for 3 h at room temperature. The mixture was then quenched with the addition of 10 mL of 1N aq. hydrochloric acid and concentrated under vacuum. The residue was diluted with THF, dried with magnesium sulfate, concentrated under vacuum and filtered through a pad of silica gel, flushing with additional THF. The resulting filtrate was concentrated under vacuum, and the residue was further purified by flash chromatography (ISCO, 12 g silica gel column, using a 0-100% ethyl acetate in n-heptane gradient as the eluent to afford 208 mg of (S)-5-cyclopropylmorpholin-3-one as a white solid (MS: (M+H)+=142.2).

後処理

  1. stirringThe resulting mixture was stirred for 3 h at room temperature
  2. customThe mixture was then quenched with the addition of 10 mL of 1N aq. hydrochloric acid
  3. concentrationconcentrated under vacuum
  4. additionThe residue was diluted with THF
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated under vacuum
  7. filtrationfiltered through a pad of silica gel
  8. customflushing with additional THF
  9. concentrationThe resulting filtrate was concentrated under vacuum
  10. customthe residue was further purified by flash chromatography (ISCO, 12 g silica gel column

出典と根拠

ORDレコード
ord-a4eca5776f324ce8801e418d483a4f8b
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697739B2

反応ノート

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