Dichloromethane → Lorazepam

HRID 1700801

반응식

HRID 1700801 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.ClCCl>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 6344DichloromethaneHCID 18318790HCID 18318790, 화합물

생성물 1

HCID 3958Lorazepam수율 97.2%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
25 °C

실험 절차

Lorazepam ethanol solvate (100 g) was suspended in a 1:1 mixture of dichloromethane and toluene (600 ml). The suspension was then heated to 25 ° C. for one hour and then cooled to 15° C. The suspension was filtered to recover the lorazepam crystals. The crystals were washed with toluene (20 ml) and dried at 50° C. under 65 mm Hg vacuum for two hours to give crystalline lorazepam (85 g, 90%)

후처리

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

출처 및 근거

ORD 기록
ord-9f8b1591cf314c2c8420f7db77e0162e
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350870B2

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