Sodium Carbonate → 6H-Pyrido(2,3-b)(1,4)benzodiazepin-6-one, 5,11-dihydro-11-((4-(3-methyl-2-butenyl)-1-piperazinyl)acetyl)-, dihydrochloride

HRID 2057979ノート

反応式

HRID 2057979 の反応式
[Cl:1][CH2:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9](=[O:16])[NH:8][C:7]2[CH:17]=[CH:18][CH:19]=[N:20][C:6]1=2)=[O:4].C(=O)([O-])[O-].[Na+].[Na+].[CH3:27][C:28]([CH3:37])=[CH:29][CH2:30][N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1>C(O)(C)C>[ClH:1].[ClH:1].[CH3:27][C:28]([CH3:37])=[CH:29][CH2:30][N:31]1[CH2:36][CH2:35][N:34]([CH2:2][C:3]([N:5]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[C:9](=[O:16])[NH:8][C:7]3[CH:17]=[CH:18][CH:19]=[N:20][C:6]2=3)=[O:4])[CH2:33][CH2:32]1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 12005311-(Chloroacetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-oneHCID 104419041-(3-Methyl-but-2-enyl)-piperazine

生成物 1

HCID 30532136H-Pyrido(2,3-b)(1,4)benzodiazepin-6-one, 5,11-dihydro-11-((4-(3-methyl-2-butenyl)-1-piperazinyl)acetyl)-, dihydrochloride

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

8.62 gm of 11-chloroacetyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]-benzodiazepin-6-one, 3.5 gm of sodium carbonate and 5.07 gm of 1-(3-methyl-but-2-enyl)-piperazine [R1 =--CH2 --CH=C(CH3)2 ] were refluxed in 100 ml of isopropanol for 2.5 hours. Then, the reaction mixture was suction-filtered while still hot, and the filtrate evaporated to a volume of 40 ml and cooled. The precipitated crystals were dissolved, while heating, in 100 ml of absolute ethanol, and the calculated quantity of concentrated hydrochloric acid was added. Upon cooling, the dihydrochloride crystallized out.

後処理

  1. filtrationThen, the reaction mixture was suction-filtered while still hot, and the filtrate
  2. customevaporated to a volume of 40 ml
  3. temperaturecooled
  4. dissolutionThe precipitated crystals were dissolved
  5. temperaturewhile heating, in 100 ml of absolute ethanol
  6. additionthe calculated quantity of concentrated hydrochloric acid was added
  7. temperatureUpon cooling
  8. customthe dihydrochloride crystallized out

出典と根拠

ORDレコード
ord-dd91e9e1335e47f69a9fe278c1c3353d
出典データセット
uspto-grants-1980_07
特許番号
US04213984

反応ノート

読み込み中…