Ethyl Acetate → Lorazepam

HRID 1700798

反応式

HRID 1700798 の反応式
[CH:1]1[CH:2]=[CH:3][C:4]([Cl:21])=[C:5]([C:7]2[C:14]3[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]=3[NH:12][C:10](=[O:11])[CH:9]([OH:20])[N:8]=2)[CH:6]=1.C(O)C.C(OCC)(=O)C>C1CCCCC1>[CH:1]1[CH:2]=[CH:3][C:4]([Cl:21])=[C:5]([C:7]2[C:14]3[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]=3[NH:12][C:10](=[O:11])[CH:9]([OH:20])[N:8]=2)[CH:6]=1

参加物

4

反応物 2

HCID 8857Ethyl AcetateHCID 18318790HCID 18318790、化合物

生成物 1

HCID 3958Lorazepam収率 97.2%

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒

反応条件

温度
60 °C

実験手順

Lorazepam ethanol solvate (100 g) was suspended in a 1:1 mixture of ethyl acetate and cyclohexane (800 ml). The suspension was heated to 60° C. for 1 hour with rapid stirring and then cooled to 15° C. The cooled suspension was filtered to recover the lorazepam crystals and the crystals were then washed with ethyl acetate (20 ml). The crystals were dried at 50° C. under 65 mm Hg vacuum for two hours to give crystalline lorazepam (85 g, 90%).

後処理

  1. temperaturecooled to 15° C
  2. filtrationThe cooled suspension was filtered
  3. customto recover the lorazepam crystals
  4. washthe crystals were then washed with ethyl acetate (20 ml)
  5. customThe crystals were dried at 50° C. under 65 mm Hg vacuum for two hours

出典と根拠

ORDレコード
ord-e77446ecc1754bb68f2c2868bde4cd7e
出典データセット
uspto-grants-2002_02
特許番号
US06350870B2

関連ノート

読み込み中…