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Tris(hydroxymethyl)aminomethane → Meloxicam trometamol

HRID 2212813
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HRID 2212813 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6503Tris(hydroxymethyl)aminomethane2회HCID 54677470Meloxicam

생성물 1

HCID 86587442Meloxicam trometamol수율 97%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-39f335226ff04835b2b1a9db5df1969f
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07105512B2

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