Lorazepam → Lormetazepam

HRID 1463969

反応式

HRID 1463969 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:22](=O)([O-])[O-].[K+].[K+].IC>CN(C)C=O>[CH3:22][N:12]1[C:10](=[O:11])[CH:9]([OH:20])[N:8]=[C:7]([C:5]2[CH:6]=[CH:1][CH:2]=[CH:3][C:4]=2[Cl:21])[C:14]2[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:13]1=2

参加物

5

反応物 3

HCID 3958LorazepamHCID 6328Methyl iodideHCID 11430Potassium Carbonate

生成物 1

HCID 13314Lormetazepam収率 98.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirring solution of lorazepam (3.21 g, 1.0×10-2 mol) in anhydrous dimethylformamide (100 ml) was added anhydrous powdered potassium carbonate (1.52 g, 1.1×10-2 mol) followed by iodomethane (0.69 ml, 1.1×10-2 mol). The mixture was stirred at room temperature for 20 hours. The solvent was evaporated under vacuum, the residue was treated with water (100 ml) and was stirred at room temperature for 2 hours. The resulting fine light yellow solid was collected by filtration and was dried under vacuum to afford 3.3 g (98%) of lormetazepam as a pale yellow solid: m.p. 201°-203° C.

後処理

  1. customThe solvent was evaporated under vacuum
  2. additionthe residue was treated with water (100 ml)
  3. stirringwas stirred at room temperature for 2 hours
  4. filtrationThe resulting fine light yellow solid was collected by filtration
  5. customwas dried under vacuum

出典と根拠

ORDレコード
ord-a0cb6a10ebc74883a8efd991da88e91a
出典データセット
uspto-grants-1994_04
特許番号
US05302715

関連ノート

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