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Methyl iodide → 4-methylsulfanyl-2-phenyl-3H-1,5-benzodiazepine

HRID 1112583
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반응식

HRID 1112583 반응식
[C:1]1([C:7]2[CH2:13][C:12](=[S:14])[NH:11][C:10]3[CH:15]=[CH:16][CH:17]=[CH:18][C:9]=3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[CH3:21]I>C1C=CC=CC=1>[CH3:21][S:14][C:12]1[CH2:13][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[N:8][C:9]2[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=2[N:11]=1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 30329842H-1,5-Benzodiazepine-2-thione, 1,3-dihydro-4-phenyl-

생성물 1

HCID 3710964-methylsulfanyl-2-phenyl-3H-1,5-benzodiazepine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

12.6 parts of 2,3-dihydro-4-phenyl-1H-1,5-benzodiazepine-2-thione is suspended in 1000 parts by volume of dry benzene. To this suspension is added 3 parts of 57% sodium hydride and the resultant mixture is stirred for about 2 hours at reflux temperature. 10 Parts of methyl iodide is then added to the reaction mixture and stirring is continued at reflux temperature overnight. The reaction mixture is then cooled to room temperature, filtered and the filtrate concentrated under reduced pressure to afford 2-methylthio-4-phenyl-3H-1,5-benzodiazepine, as an oil. This compound has the formula ##STR15##

후처리

  1. temperatureat reflux temperature
  2. temperatureat reflux temperature overnight
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a5c49148783341c58396ae4657c53380
출처 데이터셋
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04123430

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