HCID 12287603, 화합물 → 4,5-dihydro-4-(4-chlorophenyl)-2-(isopropyl)-3H-1,3,4-benzotriazepine hydrochloride

HRID 1979684노트

반응식

HRID 1979684 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][N:9]([C:11]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=1)[NH2:10].[C:18](OCC)(OCC)(OCC)[CH:19]([CH3:21])[CH3:20]>C(#N)C.Cl.CCOCC>[ClH:17].[Cl:17][C:14]1[CH:15]=[CH:16][C:11]([N:9]2[CH2:8][C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[N:1]=[C:18]([CH:19]([CH3:21])[CH3:20])[NH:10]2)=[CH:12][CH:13]=1

참가 물질

6

반응물 2

HCID 12287603HCID 12287603, 화합물HCID 133765451-[(2-Aminophenyl)methyl]-1-(4-chlorophenyl)hydrazine

생성물 1

HCID 133765634,5-dihydro-4-(4-chlorophenyl)-2-(isopropyl)-3H-1,3,4-benzotriazepine hydrochloride수율 122.8%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매

실험 절차

To a mixture of 3 g (0.012 m) of 1-[(2-aminophenyl)methyl]-1-(4-chlorophenyl)hydrazine of Example 12b and 3.56 g (0.024 m) of triethyl orthoisobutyrate in 50 ml of acetonitrile, sufficient ethereal HCl was added to make the mixture acidic. The mixture was refluxed overnight (about 16 hours), cooled and the product filtered off as the hydrochloride salt. Recrystallization by suspending the product in ethanol, adding sufficient methanol to afford a solution and diluting with anhydrous ether gave 2.5 g (62%) of 4,5-dihydro-4-(4-chlorophenyl)-2-(isopropyl)-3H-1,3,4-benzotriazepine hydrochloride, m.p. 255°-258° C.

후처리

  1. additionwas added
  2. temperatureThe mixture was refluxed overnight (about 16 hours)
  3. temperaturecooled
  4. filtrationthe product filtered off as the hydrochloride salt
  5. customRecrystallization
  6. additionadding sufficient methanol
  7. customto afford a solution

출처 및 근거

ORD 기록
ord-f0dc7745488f472ca6124f5e1482a064
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482547

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