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 2057979노트

반응식

HRID 2057979 반응식
[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

참가 물질

5

반응물 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

생성물 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

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dd91e9e1335e47f69a9fe278c1c3353d
출처 데이터셋
uspto-grants-1980_07
특허 번호
US04213984

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