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Water → HCID 15007188, 화합물

HRID 1085793
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HRID 1085793 반응식
[CH:1]([N:4]1[C:9](=[O:10])[C:8]([Br:11])=[C:7](Br)[CH:6]=[N:5]1)([CH3:3])[CH3:2].Cl.[CH3:14][O:15][C:16]1[CH:25]=[CH:24][C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]=1[CH2:26][NH2:27].C(=O)([O-])[O-].[Na+].[Na+].O>O1CCOCC1>[CH:1]([N:4]1[C:9](=[O:10])[C:8]([Br:11])=[C:7]([NH:27][CH2:26][C:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:24]=[CH:25][C:16]=2[O:15][CH3:14])[CH:6]=[N:5]1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 10827742HCID 10827742, 화합물HCID 20058940HCID 20058940, 화합물

생성물 1

HCID 15007188HCID 15007188, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture comprising 1.48 g of 2-i-propyl-4,5-dibromo-3(2H)pyridazinone, 1.68 g of 2-methoxy-1-naphthylmethylamine hydrochloride, 1.33 g of sodium carbonate, 30 ml of water and 30 ml of 1,4-dioxane, was refluxed under stirring overnight. Then, the solvent was distilled off under reduced pressure, and water was poured to the residue thus obtained. The mixture was extracted with ethyl acetate. The extract was washed sequentially with a 2 wt% hydrochloric acid aqueous solution, water and a saturated sodium chloride aqueous solution and then dried over sodium sulfate. Then, the solvent was distilled off. The residual solid thus obtained was crystallized from ethyl acetate/n-hexane to obtain 1.18 g of the above identified compound as colorless crystals having a melting point of from 160° to 161° C.

후처리

  1. temperaturewas refluxed
  2. distillationThen, the solvent was distilled off under reduced pressure, and water
  3. additionwas poured to the residue
  4. customthus obtained
  5. extractionThe mixture was extracted with ethyl acetate
  6. washThe extract was washed sequentially with a 2 wt% hydrochloric acid aqueous solution, water
  7. dry with materiala saturated sodium chloride aqueous solution and then dried over sodium sulfate
  8. distillationThen, the solvent was distilled off
  9. customThe residual solid thus obtained
  10. customwas crystallized from ethyl acetate/n-hexane
  11. customto obtain 1.18 g of the
  12. customof from 160° to 161° C.

출처 및 근거

ORD 기록
ord-0fb402eda23a412b9a550654ed8594c9
출처 데이터셋
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05011839

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