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Hydrochloric Acid → 2-Pentylcyclopentane-1,3-dione

HRID 599717
ノート
印刷プレビュー

反応式

HRID 599717 の反応式
[C:1]([OH:8])(=O)[CH2:2][CH2:3][C:4](O)=[O:5].Cl.[C:10](Cl)(=O)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]C>>[CH2:11]([CH:10]1[C:4](=[O:5])[CH2:3][CH2:2][C:1]1=[O:8])[CH2:12][CH2:13][CH2:14][CH3:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 313Hydrochloric Acid2 回HCID 1110Succinic AcidHCID 17313Heptanoyl chloride2 回

生成物 1

HCID 109428402-Pentylcyclopentane-1,3-dione

反応条件

温度
80 °C

実験手順

After charging succinic acid, the mixture was allowed stand to complete generation of HCl gas. Then, thereto was added 60 g (0.4 mol) of heptanoyl chloride, and the resulting mixture was heated at 80° C. for 8 hours. Since heptanoyl chloride is also fuming (HCl gas), measures were taken against corrosion of equipment in the peripheral environment at the time of weighing, but it was with difficulty. The mixture was cooled, poured onto 60 g of ice, and maintained at −10° C. for 10 hours, depositing a product as a solid. The product was subjected to suction filtration, washed with 10% NaCl water and toluene (20 ml×3 times), and dried, yielding 8.4 g (0.05 mol) of 2-pentyl-1,3-cyclopentanedione (a compound in which R1 represents an n-pentyl group in the above formula (3)). Yields were 20.8%, 50.0%, and 12.5% relative to AlCl3, succinic acid, and heptanoyl chloride, respectively. Simultaneously, wastewater containing a large amount of an aluminum-based and a chlorine-based compound was byproduced.

後処理

  1. temperatureThe mixture was cooled
  2. temperaturemaintained at −10° C. for 10 hours
  3. filtrationThe product was subjected to suction filtration
  4. washwashed with 10% NaCl water and toluene (20 ml×3 times)
  5. customdried

出典と根拠

ORDレコード
ord-e1246dbbaf2e437e91fe92164f5cd93e
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897802B2

反応ノート

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