Ethyl Acetate → Lorazepam

HRID 1700799

反応式

HRID 1700799 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>C1(C)C=CC=CC=1>[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 94.9%

試薬・触媒・溶媒 1

HCID 1140Toluene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 toluene (400 ml). The suspension was heated to 60° C. for 1 hour with rapid stirring and then cooled to 15° C. The suspension was filtered to recover the lorazepam. The lorazepam crystals were then washed with ethyl acetate (20 ml) and dried under 65 mm Hg vacuum at about 50° C. for about two hours to give crystalline lorazepam (83 g) in 88% yield.

後処理

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

出典と根拠

ORDレコード
ord-639a7eb95e2a4bee901453557bc86718
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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