Salbutamol → Salbutamol caprate

HRID 1383790

反応式

HRID 1383790 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].[OH:18][C:19]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[O:20]>C(O)C.C(OCC)(=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].[O-:20][C:19]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[O:18]

参加物

5

反応物 2

HCID 2083SalbutamolHCID 2969Decanoic Acid

生成物 1

HCID 86757112Salbutamol caprate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Salbutamol base (13.91 g; 58.13 mmol) was dissolved in ethanol (600 mL, 96%) with magnetic stirring to give a pale yellow liquid. Capric acid (10.01 g; 58.11 mmol) was added with vigorous stirring which was continued until all solid material had dissolved. The solvent was removed by rotary-evaporation to give a pale yellow tacky semi-solid. This was dissolved in warm ethyl acetate (300 mL), then stored at 5° C. for 36 hours, resulting in the precipitation of a fine white solid. The mother liquor was removed by vacuum filtration, and the precipitate washed with cold ethyl acetate. Any remaining solvent was removed by storing the precipitate at 35° C. and 0 bar pressure for 6 hours. Salbutamol caprate was obtained as a white solid (18.93 g; 79.13%). Moisture content K.F. 0.32%; melting point 99.4° C. (onset of endotherm in DCS thermogram). The theoretical percentage of salbutamol base in salbutamol caprate is 58.14%. Experimentally the percentage salbutamol base in salbutamol caprate was found to be 56.42%. The pH of a saturated aqueous solution is 7.24. The aqueous solubility is 4.76 mg/mL.

後処理

  1. customto give a pale yellow liquid
  2. stirringwith vigorous stirring which
  3. dissolutionhad dissolved
  4. customThe solvent was removed by rotary-evaporation
  5. customto give a pale yellow tacky semi-solid
  6. customresulting in the precipitation of a fine white solid
  7. customThe mother liquor was removed by vacuum filtration
  8. washthe precipitate washed with cold ethyl acetate
  9. customAny remaining solvent was removed
  10. customat 35° C.
  11. wait0 bar pressure for 6 hours

出典と根拠

ORDレコード
ord-b583fd131c714bd28f2c665871ba9f43
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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