Salbutamol → HCID 131722754、化合物

HRID 1383791

反応式

HRID 1383791 の反応式
[CH3:1][C:2]([NH:5][CH2:6][CH:7]([OH:17])[C:8]1[CH:9]=[CH:10][C:11]([OH:16])=[C:12]([CH2:14][OH:15])[CH:13]=1)([CH3:4])[CH3:3].[CH3:18][C@@H:19]([C@@H:29]1[C@@:33]2([CH3:49])[C@@H:34]([OH:48])[CH2:35][C@@H:36]3[C@@:41]4([CH3:47])[CH2:42][CH2:43][C@@H:44]([OH:46])[CH2:45][C@H:40]4[CH2:39][CH2:38][C@H:37]3[C@@H:32]2[CH2:31][CH2:30]1)[CH2:20][CH2:21][C:22]([NH:24][CH2:25][C:26]([OH:28])=[O:27])=[O:23].C(OCC)(=O)C>C(O)C>[CH3:4][C:2]([NH:5][CH2:6][CH:7]([OH:17])[C:8]1[CH:9]=[CH:10][C:11]([OH:16])=[C:12]([CH2:14][OH:15])[CH:13]=1)([CH3:1])[CH3:3].[CH3:18][C@@H:19]([C@@H:29]1[C@@:33]2([CH3:49])[C@@H:34]([OH:48])[CH2:35][C@@H:36]3[C@@:41]4([CH3:47])[CH2:42][CH2:43][C@@H:44]([OH:46])[CH2:45][C@H:40]4[CH2:39][CH2:38][C@H:37]3[C@@H:32]2[CH2:31][CH2:30]1)[CH2:20][CH2:21][C:22]([NH:24][CH2:25][C:26]([OH:28])=[O:27])=[O:23]

参加物

5

反応物 3

HCID 2083SalbutamolHCID 8857Ethyl Acetate2 回HCID 3035026360-65-6

生成物 1

HCID 131722754HCID 131722754、化合物収率 105.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Salbutamol base (1.2007 g; 5.02 mmol) was dissolved in ethanol (100 mL) with vigorous stirring. Glycodeoxycholic acid (2.4601 g; water content: 4.25% w/w; 5.25 mmol˜5% molar excess) was added and dissolved with stirring. A clear, colourless solution was obtained. The ethanol was removed by vacuum rotary-evaporation to give a viscous, yellow residue. Ethyl acetate (200 mL) was added to the residue and the mixture heated in a water bath with constant agitation. As the yellow residue dissolved, a white precipitate formed. Agitation was continued until the yellow residue disappeared. The ethyl acetate solution was cooled in an ice bath. The precipitate was isolated by vacuum filtration and dried in a vacuum oven at 40° C. for 20 hours to give salbutamol glycodeoxycholate (3.662 g; water content; 4.95% w/w; % yield; 97.9%). Analysis by differential scanning calorimetry from 50 to 200° C. gave no significant thermal event. Slow decomposition was evident after 110° C. A saturated aqueous solution gave a pH of 6.12. The aqueous solubility was greater than 8.35 mg/mL. The theoretical percentage of salbutamol base in the salbutamol glycodeoxycholate 34.74%.

後処理

  1. dissolutiondissolved
  2. customA clear, colourless solution was obtained
  3. customThe ethanol was removed by vacuum rotary-evaporation
  4. customto give a viscous, yellow residue
  5. temperaturethe mixture heated in a water bath with constant agitation
  6. dissolutionAs the yellow residue dissolved
  7. customa white precipitate formed
  8. customThe precipitate was isolated by vacuum filtration
  9. customdried in a vacuum oven at 40° C. for 20 hours

出典と根拠

ORDレコード
ord-2df3eac4f00b4382adc03e49033db230
出典データセット
uspto-grants-2001_07
特許番号
US06255502B1

関連ノート

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