Iodoethane → N11-Ethyl-N5-methyl-5,11-dihydro-6H-dipyrido(3,2-b:2',3'-e)(1,4)diazepin-6-one

HRID 2380226노트

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HRID 2380226 반응식
[H-].[Na+].[CH3:3][N:4]1[C:10](=[O:11])[C:9]2[CH:12]=[CH:13][CH:14]=[N:15][C:8]=2[NH:7][C:6]2[N:16]=[CH:17][CH:18]=[CH:19][C:5]1=2.[H][H].[CH2:22](I)[CH3:23]>CN(C)C=O.O>[CH2:22]([N:7]1[C:8]2[N:15]=[CH:14][CH:13]=[CH:12][C:9]=2[C:10](=[O:11])[N:4]([CH3:3])[C:5]2[CH:19]=[CH:18][CH:17]=[N:16][C:6]1=2)[CH3:23]

참가 물질

7

반응물 4

HCID 6340IodoethaneHCID 24758Sodium hydride2회HCID 148738055,11-dihydro-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-oneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 453307N11-Ethyl-N5-methyl-5,11-dihydro-6H-dipyrido(3,2-b:2',3'-e)(1,4)diazepin-6-one수율 70.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
50 °C

실험 절차

2.00 g of a 50% dispersion of sodium hydride in mineral oil was added to a solution of 5.75 g (0.025 mol) of 5,11-dihydro-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one in 100 ml of dimethylformamide. When the evolution of hydrogen ceased, the mixture was heated to 50° C. for 30 min. and then cooled to room temperature. Then, 7.80 g of ethyl iodide (neat) was added dropwise over 15 minutes, and the resulting mixture was allowed to stir overnight at room temperature. The excess sodium hydride was decomposed by the careful addition of ice, followed by water. The product was extracted with ether, dried (anhydrous sodium sulfate), and evaporated to yield 4.5 g (70% of theory) of 5,11-dihydro-11-ethyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, m.p. 130°-132° C.

후처리

  1. temperaturecooled to room temperature
  2. extractionThe product was extracted with ether
  3. dry with materialdried (anhydrous sodium sulfate)
  4. customevaporated

출처 및 근거

ORD 기록
ord-ca1957c2ce14473c88f335c2c693d765
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05366972

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