Triethylamine → N-[4-(5H-Imidazo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]-2-methylbenzamide

HRID 439968

반응식

HRID 439968 반응식
[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[C:4]([NH:6][C:7]1[CH:15]=[CH:14][C:10]([C:11](Cl)=[O:12])=[CH:9][CH:8]=1)=[O:5].C(N(CC)CC)C.[N:27]1[CH:28]=[CH:29][N:30]2[CH2:36][C:35]3[CH:37]=[CH:38][CH:39]=[CH:40][C:34]=3[NH:33][CH2:32][C:31]=12>C(Cl)Cl>[N:27]1[CH:28]=[CH:29][N:30]2[CH2:36][C:35]3[CH:37]=[CH:38][CH:39]=[CH:40][C:34]=3[N:33]([C:11]([C:10]3[CH:14]=[CH:15][C:7]([NH:6][C:4](=[O:5])[C:3]4[CH:16]=[CH:17][CH:18]=[CH:19][C:2]=4[CH3:1])=[CH:8][CH:9]=3)=[O:12])[CH2:32][C:31]=12

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 30603995H-Imidazo(2,1-c)(1,4)benzodiazepine, 10,11-dihydro-HCID 107074414-[(2-methylbenzoyl)amino]benzoyl Chloride

생성물 1

HCID 21837073N-[4-(5H-Imidazo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]-2-methylbenzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

To a mixture of 1.37 g (5 mmol) of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 15 ml of methylene chloride, cooled to 0° C. is added 1.5 ml of triethylamine. After stirring for 3 minutes, 5 mmol of 10,11-dihydro-5H-imidazo[2,1-c][1,4]benzodiazepine in 5 ml of methylene chloride is added. The cooling bath is removed and after about 30 minutes a complete solution is obtained. The reaction mixture is allowed to stir at room temperature for 1 hour and the volatiles are concentrated in vacuo. The residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, and brine. The solution is dried with Na2SO4 and the volatiles concentrated in vacuo to give the desired product as a solid.

후처리

  1. customThe cooling bath is removed and after about 30 minutes a complete solution
  2. customis obtained
  3. stirringto stir at room temperature for 1 hour
  4. concentrationthe volatiles are concentrated in vacuo
  5. dissolutionThe residue is dissolved in 100 ml of ethyl acetate
  6. washwashed with water, 2N citric acid, and brine
  7. dry with materialThe solution is dried with Na2SO4
  8. concentrationthe volatiles concentrated in vacuo

출처 및 근거

ORD 기록
ord-a431122163e447568a7b04ac3c9d729f
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05516774

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