Hydrochloric Acid → 6-Methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride

HRID 1795317ノート

反応式

HRID 1795317 の反応式
C([O:3][C:4]([C:6]1[O:7][C:8]2[C:13]([C:14](=[O:16])[CH:15]=1)=[CH:12][C:11]([O:17][CH3:18])=[CH:10][C:9]=2[N:19]1[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]1)=[O:5])C.CO.[ClH:28]>>[ClH:28].[CH3:18][O:17][C:11]1[CH:12]=[C:13]2[C:8](=[C:9]([N:19]3[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]3)[CH:10]=1)[O:7][C:6]([C:4]([OH:5])=[O:3])=[CH:15][C:14]2=[O:16]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 22142223Ethyl-6-methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylate

生成物 1

HCID 692667556-Methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride

実験手順

Ethyl-6-methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylate (1.0 g. 2.89 mmol), as prepared in Reference Example 2d above, was suspended in 6 M HCl (60 ml) and methanol (10 mL) and warmed to reflux for 3.0 h. The reaction was allowed to cool. The solution was concentrated in vacuo and anhydrous toluene was added (×3) and the solution was again concentrated in vacuo. The residue was dried under vacuum (17 h) to yield 6-methoxy-8-(4-methyl-1-piperazinyl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride as a yellow powder (1.0 g, quantitative yield).

後処理

  1. temperatureto reflux for 3.0 h
  2. temperatureto cool
  3. concentrationThe solution was concentrated in vacuo and anhydrous toluene
  4. additionwas added (×3)
  5. concentrationthe solution was again concentrated in vacuo
  6. customThe residue was dried under vacuum (17 h)

出典と根拠

ORDレコード
ord-6677715055e440ef9843ba3645e10e4e
出典データセット
uspto-grants-2006_04
特許番号
US07026314B2

反応ノート

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