Acetic Acid → HCID 10829879, 화합물

HRID 442668노트

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HRID 442668 반응식
[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][C:5]([C:15](=O)[C:16]3[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=3)=[C:6]([CH2:10][C:11](OC)=[O:12])[CH:7]=2)[O:2]1.O.[NH2:27][NH2:28].C(O)(=O)C>C(O)C>[CH2:1]1[O:2][C:3]2=[CH:4][C:5]3[C:15]([C:16]4[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=4)=[N:28][NH:27][C:11](=[O:12])[CH2:10][C:6]=3[CH:7]=[C:8]2[O:9]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 404213Methyl [6-(4-nitrobenzoyl)-2H-1,3-benzodioxol-5-yl]acetate

생성물 1

HCID 10829879HCID 10829879, 화합물수율 47.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of methyl 4,5-methylenedioxy-2-(4-nitrobenzoyl)phenylacetate (90 mg, 0.26 mmol), hydrazine hydrate (50 μL, 0.88 mmol), and acetic acid (40 μL) in ethanol (15 mL) was refluxed for 4 days. A yellow solid precipitated out from the solution. After cooling, the solvent was removed via pipette and the solid was washed with EtOAc (twice) and hexane, dried in vacuo to provide the title compound (40 mg, 47%), mp: 293°-295° C. 1H NMR (DMSO-d6) 11.2 (s, 1H), 8.31(d, 2H, J=8.8), 7.79 (d, 2H, J=8.8), 7.13 (s, 1H), 6.65 (s, 1H), 6.12 (s, 2H), 3.45 (s, 2H). Anal. Calcd. for C16H11N3O5 : C, 59.08; H, 3.41; N, 12.92. Found: C, 59.05; H, 3.43; N, 2.83.

후처리

  1. customA yellow solid precipitated out from the solution
  2. temperatureAfter cooling
  3. customthe solvent was removed via pipette
  4. washthe solid was washed with EtOAc (twice) and hexane
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-c9d4305bf88e4e86b8568995907d82c6
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891871

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