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

HRID 1979684ノート

反応式

HRID 1979684 の反応式
[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

参加物

6

反応物 2

HCID 12287603HCID 12287603、化合物HCID 133765451-[(2-Aminophenyl)methyl]-1-(4-chlorophenyl)hydrazine

生成物 1

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

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f0dc7745488f472ca6124f5e1482a064
出典データセット
uspto-grants-1984_11
特許番号
US04482547

反応ノート

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