Potassium Carbonate → HCID 22671209, 화합물

HRID 1006865노트

반응식

HRID 1006865 반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]#[C:14][C:15]1[CH:22]=[CH:21][C:20](OC)=[CH:19][C:16]=1[CH:17]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:26][OH:27].C([O-])(=O)C.[Na+].C(=O)([O-])[O-].[K+].[K+]>C(O)C.O>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[C:14]2[C:15](=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:16]=[CH:17][N+:26]=1[O-:27])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 22503528HCID 22503528, 화합물

생성물 1

HCID 22671209HCID 22671209, 화합물수율 80.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

2-[2-(4-Benzyloxybutyl)ethynyl-5-methoxybenzaldehyde (2.60 g), hydroxylamine hydrochloride (0.63 g) and sodium acetate (0.78 g) were reacted in ethanol, (30 ml) at 60° C. for 2 hr. Potassium carbonate (2.0 g) and water (5 ml) were added to the resulting reaction mixture, which was then heated under reflux for 12 hr. The reaction solution was evaporated, and the resulting residue was extracted with methylene chloride, washed with brine, and then dried. The solvent was removed and the resulting residue was purified by silica gel column chromatography (methylene chloride/methanol system), to give 2.0 g of the title compound as a brown amorphous.

후처리

  1. temperaturewas then heated
  2. temperatureunder reflux for 12 hr
  3. customThe reaction solution was evaporated
  4. extractionthe resulting residue was extracted with methylene chloride
  5. washwashed with brine
  6. customdried
  7. customThe solvent was removed
  8. customthe resulting residue was purified by silica gel column chromatography (methylene chloride/methanol system)

출처 및 근거

ORD 기록
ord-d89092ae752b4524b502804fbacc4f26
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06790844B2

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