Dexamethasone → Deltasol

HRID 926810

反応式

HRID 926810 の反応式
[CH3:1][C@H:2]1[C@:19]([OH:24])([C:20]([CH2:22][OH:23])=[O:21])[C@:18]2([CH3:25])[C@H:4]([C@H:5]3[C@:15]([F:27])([C@@H:16]([OH:26])[CH2:17]2)[C@:14]2([CH3:28])[C:8](=[CH:9][C:10]([CH:12]=[CH:13]2)=[O:11])[CH2:7][CH2:6]3)[CH2:3]1.[C:29]1(=[O:35])[O:34][C:32](=[O:33])[CH2:31][CH2:30]1>N1C=CC=CC=1.CN(C1C=CN=CC=1)C>[CH3:1][C@H:2]1[C@:19]([OH:24])([C:20]([CH2:22][O:23][C:29]([CH2:30][CH2:31][C:32]([OH:34])=[O:33])=[O:35])=[O:21])[C@:18]2([CH3:25])[C@H:4]([C@H:5]3[C@:15]([F:27])([C@@H:16]([OH:26])[CH2:17]2)[C@:14]2([CH3:28])[C:8](=[CH:9][C:10]([CH:12]=[CH:13]2)=[O:11])[CH2:7][CH2:6]3)[CH2:3]1

参加物

5

反応物 2

HCID 5743DexamethasoneHCID 7922Succinic anhydride

生成物 1

HCID 235849Deltasol

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1049Pyridine溶媒

実験手順

An amount equivalent to 0.030 g of dexamethasone (1, 0.076 mmol, 1.0 equiv.) was completely dissolved in 1 mL of pyridine (non-anhydrous) and 0.038 g of succinic anhydride (0.382 mmol, 5.0 equiv.) was added to the clear solution. Then 1-2 mg of DMAP (7.6 μmol, 0.1 equiv.) was added to the solution and reaction was allowed to run for 48 h at r.t. under N2-flow. After 48 h, pyridine was evaporated under reduced pressure (in a rotary evaporator). A volume equivalent to 10 mL of H2O was added to the evaporated residue. A white precipitate was observed which was stirred for 10 minutes and then centrifuged. The resulting precipitate was washed again with 10 mL of H2O and the washed residue was lyophilized to yield the target product (2).

後処理

  1. waitAfter 48 h
  2. custompyridine was evaporated under reduced pressure (
  3. customin a rotary evaporator)
  4. additionA volume equivalent to 10 mL of H2O was added to the evaporated residue
  5. washThe resulting precipitate was washed again with 10 mL of H2O

出典と根拠

ORDレコード
ord-2a33efbe14884b429230be4adb88a565
出典データセット
uspto-grants-2016_03
特許番号
US09289506B2

関連ノート

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