Hydrochloric Acid → HCID 54372346, 화합물

HRID 1415219노트

반응식

HRID 1415219 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 54372346HCID 54372346, 화합물수율 49%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ab0240161514a6d84555c88b5612f79
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04003936

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