3-Bromo-2,5-furandione → HCID 90419128, 화합물

HRID 530828

반응식

HRID 530828 반응식
Cl.[CH3:2][O:3][C:4]1[CH:12]=[CH:11][C:7]([CH2:8][NH:9][NH2:10])=[CH:6][CH:5]=1.[Br:13][C:14]1[C:15](=O)[O:16][C:17](=[O:19])[CH:18]=1>O>[Br:13][C:14]1[C:15](=[O:16])[N:9]([CH2:8][C:7]2[CH:11]=[CH:12][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[NH:10][C:17](=[O:19])[CH:18]=1

참가 물질

4

반응물 2

HCID 800273-Bromo-2,5-furandioneHCID 457893744-Methoxybenzylhydrazine hydrochloride

생성물 1

HCID 90419128HCID 90419128, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

(4-methoxybenzyl)hydrazine hydrochloride (2.132 g, 11.30 mmol) and 3-bromofuran-2,5-dione (2 g, 11.30 mmol) in water (20 ml) was stirred and heated at 100° C. overnight. The mixture was cooled to room temperature and filtered to collect the solid. The solid was triturated with a mixture of ethyl acetate and ethyl ether (1/4) and the mixture was filtered. The insoluble residue was 4-bromo-1-(4-methoxybenzyl)-1,2-dihydropyridazine-3,6-dione. LRMS m/z (M+H) 311.0 found, 311.0 required. The filtrate was concentrated in vacuo and the residue was purified by column chromatography on silica gel (Petroleum ether: ethyl acetate=1/1)) to give 5-bromo-1-(4-methoxybenzyl)-1,2-dihydropyridazine-3,6-dione. LRMS m/z (M+H) 311.0 found, 311.0 required.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered
  3. customto collect the solid
  4. customThe solid was triturated with a mixture of ethyl acetate and ethyl ether (1/4)
  5. filtrationthe mixture was filtered
  6. concentrationThe filtrate was concentrated in vacuo
  7. customthe residue was purified by column chromatography on silica gel (Petroleum ether: ethyl acetate=1/1))

출처 및 근거

ORD 기록
ord-1d7cd40a9392450cbe486614f9434826
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353104B2

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