Hydrochloric Acid → HCID 56926625、化合物

HRID 1040297ノート

反応式

HRID 1040297 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:8](=[O:11])[CH2:9][CH3:10])[CH:5]=[CH:6][CH:7]=1.[CH2:12]=O.Cl.[CH3:15][NH:16][CH3:17].Cl>O.C(O)(C)C>[CH3:15][N:16]([CH3:17])[CH2:10][CH:9]([CH3:12])[C:8]([C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([OH:1])[CH:3]=1)=[O:11]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 831413'-Hydroxypropiophenone

生成物 1

HCID 56926625HCID 56926625、化合物収率 55.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3776Isopropanol溶媒

反応条件

温度
27.5 °C

実験手順

A mixture of 1-(3-hydroxy-phenyl)-propan-1-one (5 g, 0.03 mol), paraformaldehyde (1 g, 0.03 mol), dimethylamine hydrochloride (3 g, 0.04 mol), hydrochloric acid (3.4 ml, 30%) and isopropanol (15 ml) was refluxed for 16 hours. Isopropanol was distilled off from the reaction mixture and resulting reaction mass was cooled to 25-30° C. Water (15 ml) was added to the reaction mass and washed with isopropyl ether (2×15 ml). Layers were separated and aqueous layer was added to a stirred mixture of aqueous sodium hydroxide solution (1.2 g in 16 ml water) and methyl tert-butyl ether (25 ml). Layers were separated. Organic layer was washed with water (10 ml), dried and solvent was distilled to give 3.45 g of the title compound.

後処理

  1. temperaturewas refluxed for 16 hours
  2. distillationIsopropanol was distilled off from the reaction mixture
  3. customresulting
  4. customreaction mass
  5. washwashed with isopropyl ether (2×15 ml)
  6. customLayers were separated
  7. additionaqueous layer was added to a stirred mixture of aqueous sodium hydroxide solution (1.2 g in 16 ml water) and methyl tert-butyl ether (25 ml)
  8. customLayers were separated
  9. washOrganic layer was washed with water (10 ml)
  10. customdried
  11. distillationsolvent was distilled

出典と根拠

ORDレコード
ord-90bebda661f9416ab7c930a73907b21f
出典データセット
uspto-grants-2013_10
特許番号
US08552219B2

反応ノート

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