Lorazepam methanol → Lorazepam

HRID 1700802

反応式

HRID 1700802 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.CO>C(OCC)(=O)C>[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

3

反応物 1

HCID 18318792Lorazepam methanol

生成物 1

HCID 3958Lorazepam収率 93.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

Lorazepam methanol solvate (100 g) was suspended in ethyl acetate (400 ml). The suspension was heated to 60° C. for one hour with rapid stirring and then cooled to 15° C. The suspension was filtered to recover the lorazepam crystals. The crystals were washed with ethyl acetate (50 ml) and dried at 50° C. under 65 mm Hg vacuum for two hours to give crystalline lorazepam (85 g, 80%).

後処理

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

出典と根拠

ORDレコード
ord-a81d3a8696ed4d79bd8815cdfa0665d2
出典データセット
uspto-grants-2002_02
特許番号
US06350870B2

関連ノート

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