Water → Pyrazolo(4,3-e)pyrido(3,2-b)(1,4)diazepin-10(1H)-one, 4,9-dihydro-1,3,9-trimethyl-

HRID 1702439노트

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HRID 1702439 반응식
[CH3:1][N:2]1[C:11]2[C:10](=[O:12])[NH:9][C:8]3[CH:13]=[CH:14][CH:15]=[N:16][C:7]=3[NH:6][C:5]=2[C:4]([CH3:17])=[N:3]1.[H-].[Na+].[CH3:20]I.O>CN(C)C=O>[CH3:1][N:2]1[C:11]2[C:10](=[O:12])[N:9]([CH3:20])[C:8]3[CH:13]=[CH:14][CH:15]=[N:16][C:7]=3[NH:6][C:5]=2[C:4]([CH3:17])=[N:3]1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 3069939Pyrazolo(4,3-e)pyrido(3,2-b)(1,4)diazepin-10(1H)-one, 4,9-dihydro-1,3-dimethyl-

생성물 1

HCID 3069940Pyrazolo(4,3-e)pyrido(3,2-b)(1,4)diazepin-10(1H)-one, 4,9-dihydro-1,3,9-trimethyl-

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

An amount of 5.25 gm (0.025 mol) of 1,3-dimethyl-1,4,9,10-tetrahydro-pyrazolo[4,3-e]pyrido[3,2-b][1,4]diazepin-10-one was dissolved in 25 ml of N,N-dimethylformamide and mixed with 1.2 gm of a 55% sodium hydride dispersion in mineral oil. After stirring for 2 hours at 60° C., the solution was cooled to 40° C., and 2.2 ml of methyl iodide were added dropwise. Subsequently the mixture was stirred for 3 hours at 40° C., and after addition of 50 ml of water and cooling in the ice-bath, the desired compound was obtained in crystals. The crystals were recovered by suction filtration, and the mineral oil was washed out by means of petroleum ether.

후처리

  1. temperaturethe solution was cooled to 40° C.
  2. stirringSubsequently the mixture was stirred for 3 hours at 40° C.

출처 및 근거

ORD 기록
ord-48ec64fca1f34e6c9d3739b1b6b48e44
출처 데이터셋
uspto-grants-1983_04
특허 번호
US04381303

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