Triethylamine → N-[4-(4H-Furo[2,3-e]pyrrolo[1,2-a][1,4]-diazepin-10(9H)-ylcarbonyl)phenyl]-2-methyl benzamide

HRID 1420002노트

반응식

HRID 1420002 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.[O:27]1[C:31]2[NH:32][CH2:33][C:34]3[N:35]([CH:37]=[CH:38][CH:39]=3)[CH2:36][C:30]=2[CH:29]=[CH:28]1>C(Cl)Cl>[O:27]1[C:31]2[N:32]([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])[CH2:33][C:34]3[N:35]([CH:37]=[CH:38][CH:39]=3)[CH2:36][C:30]=2[CH:29]=[CH:28]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 107074414-[(2-methylbenzoyl)amino]benzoyl ChlorideHCID 218369669,10-Dihydro-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine

생성물 1

HCID 21837211N-[4-(4H-Furo[2,3-e]pyrrolo[1,2-a][1,4]-diazepin-10(9H)-ylcarbonyl)phenyl]-2-methyl benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a mixture of 1.1 mmol of 4-[(2-methylbenzoyl)amino]benzoyl chloride in 10 ml of methylene chloride, cooled to 0° C. is added 1.5 mmol of triethylamine. To the mixture is added 1 mmol of 9,10-dihydro-4H-furo[2,3-e]pyrrolo[1,2-a][1,4]diazepine and the mixture stirred at room temperature for 2 hours. The reaction mixture is concentrated in vacuo and the residue is dissolved in 100 ml of ethyl acetate and washed with water, 2N citric acid, aqueous NaHCO3 and brine. The solution is dried with Na2SO4 and the volatiles concentrated in vacuo to give a solid which is purified by flash chromatography to give the desired product.

후처리

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. dissolutionthe residue is dissolved in 100 ml of ethyl acetate
  3. washwashed with water, 2N citric acid, aqueous NaHCO3 and brine
  4. dry with materialThe solution is dried with Na2SO4
  5. concentrationthe volatiles concentrated in vacuo
  6. customto give a solid which
  7. customis purified by flash chromatography

출처 및 근거

ORD 기록
ord-c593577e214a4a958805a8689975652a
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05889001

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