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Methylamine → HCID 44265477, 화합물

HRID 1451273
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HRID 1451273 반응식
CN.[CH2:3]([N:5](CC)CC)C.[N+:10]([C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:25]3[CH:26]=[C:27]4[O:32][CH2:31][O:30][C:28]4=[CH:29][C:24]=3[CH2:23][CH:22]([CH3:33])[N:21]([C:34](=[O:37])[CH2:35]Cl)[N:20]=2)=[CH:15][CH:14]=1)([O-])=O>C(O)C>[NH2:10][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[C:25]3[CH:26]=[C:27]4[O:32][CH2:31][O:30][C:28]4=[CH:29][C:24]=3[CH2:23][CH:22]([CH3:33])[N:21]([C:34](=[O:37])[CH2:35][NH:5][CH3:3])[N:20]=2)=[CH:15][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6329MethylamineHCID 8471TriethylamineHCID 11090693HCID 11090693, 화합물

생성물 1

HCID 44265477HCID 44265477, 화합물수율 53.6%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.03 g (15.3 mmol) of methylamine hydrocdhloride and 2.64 ml (18.3 mmol) of triethylamine were added to a suspension containing 1.23 g (3.06 mmol) of 1-(4-nitrophenyl)-3-chloroacetyl-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine in 140 ml of ethanol and the reaction mixture was refluxed for 10hours, then evaporated under reduced pressure. The residue was dissolved in 30 ml of chloroform, washed with 20 ml of 4% NaOH solution, then 2×20 ml of water, dried and evaporated under reduced pressure. The residue was reduced according to the process of Example 16 and the product obtained was purified by column chromatography (adsorbent: Kieselgel 60, eluent: methanol--benzene 4:1). The crude product obtained was triturated with 5 ml of ethyl acetate at 25 ° C. to obtain 0.60 g (53.6%) of the aimed product, m.p. 198°-200° C. (weak decomp.).

후처리

  1. temperaturethe reaction mixture was refluxed for 10hours
  2. customevaporated under reduced pressure
  3. dissolutionThe residue was dissolved in 30 ml of chloroform
  4. washwashed with 20 ml of 4% NaOH solution
  5. dry with material2×20 ml of water, dried
  6. customevaporated under reduced pressure
  7. customthe product obtained
  8. customwas purified by column chromatography (adsorbent: Kieselgel 60, eluent: methanol--benzene 4:1)
  9. customThe crude product obtained
  10. customwas triturated with 5 ml of ethyl acetate at 25 ° C.

출처 및 근거

ORD 기록
ord-8c015a307c764de2bb5731e6a9dee2c6
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05604223

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