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Hexamethylenetetramine → HCID 19858062、化合物

HRID 2073387
ノート
印刷プレビュー

反応式

HRID 2073387 の反応式
[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]
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 3

HCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 19858068HCID 19858068、化合物

生成物 1

HCID 19858062HCID 19858062、化合物

実験手順

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.

後処理

temperature
under 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
  • 出典と根拠

    ORDレコード
    ord-37837a46ffaf41399e01530dd358d1aa
    出典データセット
    uspto-grants-1990_04
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04916148

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