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Hexamethylenetetramine → HCID 19858062, 화합물

HRID 2073387
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HRID 2073387 반응식
[CH3:1][C:2]1([CH3:17])[C:6](=[O:7])[O:5][C:4]2[CH:8]=[CH:9][C:10]3[C:15]([C:3]1=2)=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=3.FC(F)(F)[C:20](O)=[O:21].C1N2CN3CN(C2)CN1C3>>[CH:20]([C:12]1[CH:11]=[C:10]2[C:15](=[CH:14][C:13]=1[CH3:16])[C:3]1[C:2]([CH3:17])([CH3:1])[C:6](=[O:7])[O:5][C:4]=1[CH:8]=[CH:9]2)=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 19858068HCID 19858068, 화합물

생성물 1

HCID 19858062HCID 19858062, 화합물

실험 절차

A mixture of 1,1,8-trimethyl-2-(1H)-naphtho[2,1-b]furanone (3.85)g, trifluoracetic acid (25 ml) and hexamine (3.5 g) was stirred under reflux for 18 h. The bulk of the trifluoroacetic acid was evaporated under reduced pressure and the residue was treated with water and heated at 90° for 10 minutes. The mixture was neutralised with potassium hydrogen carbonate and extracted twice with chloroform. The combined extracts were dried and evaporated to dryness, and the residue was recrystallised from ethyl acetate to give 7-formyl-1,1,8-trimethyl-2(1H)-naphtho[2,1-b]furanone (2.2 g), m.p. 193°-195° C.

후처리

  • temperatureunder reflux for 18 h
  • customThe bulk of the trifluoroacetic acid was evaporated under reduced pressure
  • additionthe residue was treated with water
  • temperatureheated at 90° for 10 minutes
  • extractionextracted twice with chloroform
  • customThe combined extracts were dried
  • customevaporated to dryness
  • customthe residue was recrystallised from ethyl acetate
  • 출처 및 근거

    ORD 기록
    ord-37837a46ffaf41399e01530dd358d1aa
    출처 데이터셋
    uspto-grants-1990_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04916148

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