Hydrochloric Acid → HCID 68670524, 화합물

HRID 2389859

반응식

HRID 2389859 반응식
[Cl:1][C:2]1[C:11]2[C:12]3[C:17]([NH:18][C:10]=2[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1)=[CH:16][CH:15]=[CH:14][CH:13]=3.N1C2C(=CC=CC=2)C(=O)C1=O.[OH:30][CH2:31][CH2:32][NH:33][CH2:34][CH2:35][NH2:36].Cl>C(OCCO)C.CC(=O)OCC.CO>[ClH:1].[CH:8]1[CH:7]=[CH:6][CH:5]=[C:4]2[C:9]=1[C:10]1[NH:18][C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11]=1[C:2]([NH:36][CH2:35][CH2:34][NH:33][CH2:32][CH2:31][OH:30])=[N:3]2

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 7054IsatinHCID 8112N-(2-Hydroxyethyl)ethylenediamineHCID 54103076-Chloro-11H-indolo[3,2-c]quinoline

생성물 1

HCID 68670524HCID 68670524, 화합물수율 70%

시약·촉매·용매 3

HCID 887Methanol용매HCID 8076Glycol monoethyl ether용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of compound 4a as obtained from the above Synthesis Ex. 1 (0.50 g, 2 mmol) and N-(2-hydroxyethyl)ethylenediamine (0.63 g, 6 mmol) in 2-ethoxyethanol (5 mL) was heated at 140-150° C. for 24 hrs (by TLC monitoring). After cooling, the reaction mixture was evaporated in vacuo to give a residue, which was dissolved in EA (50 mL). The EA layer was washed with H2O and brine and then dried (MgSO4). Concentration of the EA layer gave a residue, which was dissolved in MeOH (10 mL) and then added with a solution of 6N HCl at 0° C., followed by stirring at room temperature for 8 hrs. The resultant precipitate was filtered off, washed with MeOH, and dried at 90° C. under reduced pressure for 24 hrs to give the title compound 9 (0.50 g, 70% yield).

후처리

  1. customas obtained from the above Synthesis Ex
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated in vacuo
  4. customto give a residue, which
  5. washThe EA layer was washed with H2O and brine
  6. dry with materialdried (MgSO4)
  7. customConcentration of the EA layer gave a residue, which
  8. filtrationThe resultant precipitate was filtered off
  9. washwashed with MeOH
  10. customdried at 90° C. under reduced pressure for 24 hrs

출처 및 근거

ORD 기록
ord-4f8e9553cc7d47a1a546fd042eb9d488
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273760B2

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