Ethyl Acetate → Lorazepam

HRID 1700799

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HRID 1700799 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(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

참가 물질

4

반응물 2

HCID 8857Ethyl AcetateHCID 18318790HCID 18318790, 화합물

생성물 1

HCID 3958Lorazepam수율 94.9%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-639a7eb95e2a4bee901453557bc86718
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350870B2

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