Acetic Acid → HCID 178433874, 화합물

HRID 59619

반응식

HRID 59619 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12](=[N:15][NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([Br:23])[C:18]=3[O:24]C)[C:11]([CH3:26])=[N:10]2)[CH:5]=[CH:6][C:7]=1[CH3:8].C(O)(=O)C.O.C(=O)(O)[O-].[Na+]>Br>[CH3:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13](=[O:14])[C:12](=[N:15][NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([Br:23])[C:18]=3[OH:24])[C:11]([CH3:26])=[N:10]2)[CH:5]=[CH:6][C:7]=1[CH3:8]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 1784863784-[(3-bromo-2-methoxyphenyl)hydrazinylidene]-2-(3,4-dimethylphenyl)-5-methylpyrazol-3-one

생성물 1

HCID 178433874HCID 178433874, 화합물

시약·촉매·용매 1

HCID 260Hydrogen Bromide용매

실험 절차

A solution of 1-(3,4-dimethylphenyl)-3-methyl-4-(3-bromo-2-methoxyphenyl)hydrazono-5-pyrazolone(5 g) prepared as in Example 2, in 48% aqueous hydrobromic acid (200 mL) and glacial acetic acid (50 mL) was stirred and heated under reflux for about 80 hours. The reaction mixture was concentrated under vacuum to obtain a thick residue. Water (40 mL) was added and basified to pH 7-8 using saturated solution of sodium bicarbonate (20 mL). The mixture was filtered to give an orange solid, which was washed with water (25 mL) and dried in an oven at about 55° C. to about 60° C. for about 12 hours. Yield: 3.5 g

후처리

  1. temperatureheated
  2. temperatureunder reflux for about 80 hours
  3. concentrationThe reaction mixture was concentrated under vacuum
  4. customto obtain a thick residue
  5. filtrationThe mixture was filtered
  6. customto give an orange solid, which
  7. washwas washed with water (25 mL)
  8. customdried in an oven at about 55° C. to about 60° C. for about 12 hours

출처 및 근거

ORD 기록
ord-192beb1209844b92a742a2d9f4b045d0
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440927B2

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