Dimethylformamide → 4,9-Dihydro-9-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

HRID 436146노트

반응식

HRID 436146 반응식
[CH:1]1[S:2][CH:3]=[C:4]2[C:10]=1[C:9](=[O:11])[NH:8][C:7]1[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=1[NH:5]2.[H-].[Na+].[CH3:18]N(C)C=O.CI>O>[CH3:18][N:8]1[C:7]2[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=2[NH:5][C:4]2=[CH:3][S:2][CH:1]=[C:10]2[C:9]1=[O:11]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 125216414,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

생성물 1

HCID 203922504,9-Dihydro-9-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of 0.84 g. of 4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 0.18 g. of 55% sodium hydride-mineral oil dispersion in 25 ml. of dimethylformamide is added 0.3 ml. of methyl iodide. The reaction mixture is stirred for 2.5 hours, cooled, diluted with water and filtered. The solid product is recrystallized from methanol-water to give pale yellow crystals, m.p. 195°-198° C.

후처리

  1. additionTo a stirred mixture of 0.84 g
  2. temperaturecooled
  3. filtrationfiltered
  4. customThe solid product is recrystallized from methanol-water
  5. customto give pale yellow crystals, m.p. 195°-198° C.

출처 및 근거

ORD 기록
ord-464a81f81d234e15b9bf668e99004aa4
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04007272

반응 노트

불러오는 중…