Lorazepam → Lormetazepam

HRID 1463969

반응식

HRID 1463969 반응식
[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

참가 물질

5

반응물 3

HCID 3958LorazepamHCID 6328Methyl iodideHCID 11430Potassium Carbonate

생성물 1

HCID 13314Lormetazepam수율 98.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a0cb6a10ebc74883a8efd991da88e91a
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05302715

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