Hydrochloric Acid → HCID 54027579、化合物

HRID 1415221ノート

反応式

HRID 1415221 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].[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]

参加物

7

反応物 4

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

生成物 1

HCID 54027579HCID 54027579、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 (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.

後処理

  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

出典と根拠

ORDレコード
ord-8cbf869a563a4bb1b4da9f57ce09c35f
出典データセット
uspto-grants-1977_01
特許番号
US04003936

反応ノート

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