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Dimethylamine → HCID 15615542、化合物

HRID 1194319
ノート
印刷プレビュー

反応式

HRID 1194319 の反応式
[C:1]([C:4]1[O:8][C:7]([C:9](Cl)=[O:10])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[CH3:12][NH:13][CH3:14]>O1CCCC1>[CH3:12][N:13]([CH3:14])[C:9]([C:7]1[O:8][C:4]([C:1](=[O:3])[CH3:2])=[CH:5][CH:6]=1)=[O:10]
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 674DimethylamineHCID 156155415-Acetylfuran-2-carbonyl chloride

生成物 1

HCID 15615542HCID 15615542、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 9.1 g. (0.053 mole) of 5-acetylfuran-2-carbonyl chloride in 150 ml. of tetrahydrofuran at ca -30° C. was added, dropwise, 7.0 ml. (0.106 mole) of dimethylamine. Stirring was continued, and the reaction mixture was allowed to warm to room temperature and then stirred overnight. The tetrahydrofuran was removed by evaporation in vacuo, and the residue was diluted with water and extracted with ethyl acetate. The extracts were washed with water, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography on silica gel, eluting with 1:20 methanol-chloroform, to give 7.33 g. of the title compound as a solid, mp 101°-104° C. A small sample was recrystallized from cyclohexane to give a pale yellow solid, mp. 104°-106° C.

後処理

  1. stirringstirred overnight
  2. customThe tetrahydrofuran was removed by evaporation in vacuo
  3. additionthe residue was diluted with water
  4. extractionextracted with ethyl acetate
  5. washThe extracts were washed with water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by chromatography on silica gel
  9. washeluting with 1:20 methanol-chloroform
  10. customto give 7.33 g

出典と根拠

ORDレコード
ord-79d3b29750484b60b21e5f529f31bad2
出典データセット
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04814341

反応ノート

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