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Methyl Isocyanate → HCID 18975136, 화합물

HRID 2393490
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HRID 2393490 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][NH:9][CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1.[CH3:23][N:24]=[C:25]=[O:26]>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[C:11]([C:12]3[CH:13]=[CH:14][C:15]([N+:18]([O-:20])=[O:19])=[CH:16][CH:17]=3)=[N:10][N:9]([C:25](=[O:26])[NH:24][CH3:23])[CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 11023487HCID 11023487, 화합물

생성물 1

HCID 18975136HCID 18975136, 화합물수율 95.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.72 g (2.2 mmoles) of 7-chloro-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine prepared in Example 1, Step D are dissolved in 15 ml of anhydrous dichloromethane, and to the solution obtained, 1.3 ml (22.0 moles) of methyl isocyanate are added, and the reaction mixture is left to stand at 25° C. for 10 days. The mixture is evaporated, and the residue is recrystallized from 3 ml of hot ethanol. The crystals are filtered, washed 3 times using 1 ml of ethanol each time, then dried. Thus, 0.78 g (95%) of the title compound are obtained. M.p.: 224°-226° C.

후처리

  1. customto the solution obtained
  2. waitthe reaction mixture is left
  3. customThe mixture is evaporated
  4. customthe residue is recrystallized from 3 ml of hot ethanol
  5. filtrationThe crystals are filtered
  6. washwashed 3 times
  7. customdried

출처 및 근거

ORD 기록
ord-2d8952085b0444ad85322094f7fb7994
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05807851

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