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Tris(hydroxymethyl)aminomethane → Meloxicam trometamol

HRID 2212813
ノート
印刷プレビュー

反応式

HRID 2212813 の反応式
[NH2:1][C:2]([CH2:7][OH:8])([CH2:5][OH:6])[CH2:3][OH:4].[CH3:9][C:10]1[S:14][C:13]([NH:15][C:16]([C:18]2[N:29]([CH3:30])[S:26](=[O:28])(=[O:27])[C:25]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:19]=2[OH:31])=[O:17])=[N:12][CH:11]=1>C(O)C>[CH3:9][C:10]1[S:14][C:13]([NH:15][C:16]([C:18]2[N:29]([CH3:30])[S:26](=[O:27])(=[O:28])[C:25]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:19]=2[OH:31])=[O:17])=[N:12][CH:11]=1.[NH2:1][C:2]([CH2:7][OH:8])([CH2:5][OH:6])[CH2:3][OH:4]
参加物反応条件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 6503Tris(hydroxymethyl)aminomethane2 回HCID 54677470Meloxicam

生成物 1

HCID 86587442Meloxicam trometamol収率 97%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

To 0.4 L of ethanol, there was added 2.42 g (20 mM) of trometamol and the resulting mixture was heated to 80° C. To the resulting trometamol solution, there was added 7.03 g (20 mM) of meloxicam and the resulting mixture was stirred for one hour, while maintaining the temperature of the mixture at 80° C. The solution was filtered while it was still hot, cooled to room temperature and then concentrated to dryness under reduced pressure. Cold ethanol (100 mL) was added to the resulting yellow solid residue and then the solid mass of the residue was triturated. The precipitates were subjected to suction filtration and the resulting crystalline powder was dried under reduced pressure to give 9.13 g (yield 97%) of meloxicam trometamol salt.

後処理

  1. temperaturewhile maintaining the temperature of the mixture at 80° C
  2. filtrationThe solution was filtered while it
  3. temperaturecooled to room temperature
  4. concentrationconcentrated to dryness under reduced pressure
  5. additionCold ethanol (100 mL) was added to the resulting yellow solid residue
  6. customthe solid mass of the residue was triturated
  7. filtrationThe precipitates were subjected to suction filtration
  8. customthe resulting crystalline powder was dried under reduced pressure

出典と根拠

ORDレコード
ord-39f335226ff04835b2b1a9db5df1969f
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07105512B2

反応ノート

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