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Ethyl 4-[(1,1-dimethylethyl)(2-ethoxy-2-oxoethyl)amino]butanoate → HCID 22228430、化合物

HRID 1744693
ノート
印刷プレビュー

反応式

HRID 1744693 の反応式
[C:1]([N:5]([CH2:14][C:15]([O:17]CC)=O)[CH2:6][CH2:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])([CH3:4])([CH3:3])[CH3:2].CC(C)([O-])C.[K+]>O1CCCC1>[C:1]([N:5]1[CH2:6][CH2:7][CH:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:15](=[O:17])[CH2:14]1)([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 22228401Ethyl 4-[(1,1-dimethylethyl)(2-ethoxy-2-oxoethyl)amino]butanoateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 22228430HCID 22228430、化合物収率 61.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of the product of step B (14.0 g; 50.9 mmol) in tetrahydrofuran (200 mL) was added 1.05 eq of potassium tert-butoxide (6.0 g; 53.5 mmol). The reaction was maintained at ambient temperature for 2 h and then quenched with a sufficient amount of saturated aqueous ammonium chloride to make the solution pH 8. The tetrahydrofuran was removed in vacuo and the aqueous layer was extracted three times with diethyl ether. The combined organic extracts were washed with brine, dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound (7.15 g).

後処理

  1. customquenched with a sufficient amount of saturated aqueous ammonium chloride
  2. customThe tetrahydrofuran was removed in vacuo
  3. extractionthe aqueous layer was extracted three times with diethyl ether
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f62717219e7540b8919ef7568fe0faab
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07015235B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート