Hydrochloric Acid → HCID 54027579, 화합물

HRID 1415221노트

반응식

HRID 1415221 반응식
[C:1]([CH:4]1[C:8](=[O:9])[CH2:7][CH2:6][C:5]1=[O:10])(=[O:3])[CH3:2].[OH:11][C:12]1[C:19]([O:20][CH3:21])=[CH:18][CH:17]=[CH:16][C:13]=1[CH:14]=O.N1CCOCC1.Cl>O.CS(C)=O>[OH:11][C:12]1[C:19]([O:20][CH3:21])=[CH:18][CH:17]=[CH:16][C:13]=1[CH:14]=[CH:2][C:1]([CH:4]1[C:8](=[O:9])[CH2:7][CH2:6][C:5]1=[O:10])=[O:3]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8083MorpholineHCID 8991o-VanillinHCID 3364732-Acetyl-1,3-cyclopentanedione

생성물 1

HCID 54027579HCID 54027579, 화합물수율 49%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

2-Acetyl-1,3-cyclopentanedione (4.26 g.) was treated with 4.94 g. of 2-hydroxy-3-methoxybenzaldehyde in 100 ml. of dimethylsulfoxide in the presence of 6 ml. of morpholine at 85° C for 40 minutes. After cooling, the reaction mixture was poured into 300 ml. of water containing 12 ml. of conc. hydrochloric acid. Deposited crystals were separated by filtration and washed with water, and dried. 2-(2-Hydroxy-3-methoxycinnamoyl)-1,3-cyclopentanedione (4.40 g., 49%) was obtained in yellow crystalline state, which showed mp. 198° - 200° C. after recrystallization from a mixed solvent of dioxane and ethanol.

후처리

  1. temperatureAfter cooling
  2. additionthe reaction mixture was poured into 300 ml
  3. customDeposited crystals were separated by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-8cbf869a563a4bb1b4da9f57ce09c35f
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04003936

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