Hydrochloric Acid → HCID 54372346、化合物

HRID 1415219ノート

反応式

HRID 1415219 の反応式
[C:1]([CH:4]1[C:8](=[O:9])[CH2:7][CH2:6][C:5]1=[O:10])(=[O:3])[CH3:2].[CH:11]1[C:16]([CH:17]=O)=[CH:15][C:14]2[O:19][CH2:20][O:21][C:13]=2[CH:12]=1.N1CCOCC1.Cl>O.CS(C)=O>[CH2:20]1[O:21][C:13]2[CH:12]=[CH:11][C:16]([CH:17]=[CH:2][C:1]([CH:4]3[C:8](=[O:9])[CH2:7][CH2:6][C:5]3=[O:10])=[O:3])=[CH:15][C:14]=2[O:19]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8083MorpholineHCID 8438PiperonalHCID 3364732-Acetyl-1,3-cyclopentanedione

生成物 1

HCID 54372346HCID 54372346、化合物収率 49%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

2-Acetyl-1,3-cyclopentanedione (3.39 g.) was treated with piperonal (4.79 g.) in 60 ml. of dimethylsulfoxide in the presence of 5 ml. of morpholine at 85° C for 45 minutes. After cooling, the reaction mixture was poured into 150 ml. of water containing 7 ml. of conc. hydrochloric acid. Deposited crystals were separated by filtration and washed with water, and dried. 2-(3,4-Methylenedioxycinnamoyl)-1,3-cyclopentanedione (3.23 g.) was obtained in a yellow crystalline form, which showed mp. 181° - 182° C. after recrystallization from a mixed solvent of dioxane and ethanol.

後処理

  1. temperatureAfter cooling
  2. additionthe reaction mixture was poured into 150 ml
  3. customDeposited crystals were separated by filtration
  4. washwashed with water
  5. customdried

出典と根拠

ORDレコード
ord-6ab0240161514a6d84555c88b5612f79
出典データセット
uspto-grants-1977_01
特許番号
US04003936

反応ノート

読み込み中…