Potassium Carbonate → HCID 22671209、化合物

HRID 1006865ノート

反応式

HRID 1006865 の反応式
[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

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 22503528HCID 22503528、化合物

生成物 1

HCID 22671209HCID 22671209、化合物収率 80.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-d89092ae752b4524b502804fbacc4f26
出典データセット
uspto-grants-2004_09
特許番号
US06790844B2

反応ノート

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