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Dimethylamine → HCID 15615542, 화합물

HRID 1194319
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HRID 1194319 반응식
[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]
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참가 물질

4

반응물 2

HCID 674DimethylamineHCID 156155415-Acetylfuran-2-carbonyl chloride

생성물 1

HCID 15615542HCID 15615542, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-79d3b29750484b60b21e5f529f31bad2
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04814341

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