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Water → 2-(4-chlorophenyl)-N-[1-methyl-1-isopropyl-2-oxopropyl]propanamide

HRID 992762
ノート
印刷プレビュー

反応式

HRID 992762 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:10]2[O:11][C:12](=[O:19])[C:13]([CH:16]([CH3:18])[CH3:17])([CH3:15])[N:14]=2)[CH3:9])=[CH:4][CH:3]=1.C[Li].[CH3:22]COCC.C(OCC)(=O)C.O>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:9])[C:10]([NH:14][C:13]([CH3:15])([CH:16]([CH3:18])[CH3:17])[C:12](=[O:19])[CH3:22])=[O:11])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 113120132-[1-(4-Chlorophenyl)ethyl]-4-isopropyl-4-methyl-1,3-oxazol-5-oneHCID 178467906HCID 178467906、化合物

生成物 1

HCID 114833132-(4-chlorophenyl)-N-[1-methyl-1-isopropyl-2-oxopropyl]propanamide収率 55.6%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

4.8 g (18 mmol) of 2-[1-(4-chlorophenyl)ethyl]-4-isopropyl-4-methyl-1,3-oxazol-5-one was dissolved in 40 ml of tetrahydrofuran. Thereto was dropwise added, at 5° C., a solution obtained by diluting 20.4 ml of a 1.14 M/liter methyllithium ether solution (23.3 mmol) with 50 ml of tetrahydrofuran. The mixture was kept at 10° C. or below and subjected to a reaction for 1 hour. After the completion of the reaction, ethyl acetate and water were added for phase separation. The separated organic layer was concentrated. The resulting concentrate was subjected to column chromatography to obtain 2.9 g (0.01 mol) (yield=55%) of 2-(4-chlorophenyl)-N-[1-methyl-1-isopropyl-2-oxopropyl]propanamide.

後処理

  1. additionThereto was dropwise added, at 5° C.
  2. customa solution obtained
  3. customwas kept at 10° C. or below
  4. customsubjected to a reaction for 1 hour
  5. additionwere added for phase separation
  6. concentrationThe separated organic layer was concentrated
  7. concentrationThe resulting concentrate

出典と根拠

ORDレコード
ord-8f6e24c9241d4a908cb2d6ebe592f737
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06469210B1

反応ノート

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