1,2-Dichloroethane → HCID 22404520、化合物

HRID 259982ノート

反応式

HRID 259982 の反応式
[Cl:1][C:2](CCl)=[CH2:3].[C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])[CH3:7].[CH2:15](Cl)CCl>[Zn].C(O)(=O)C>[Cl:1][C:2]([CH2:7][C:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)([OH:8])[CH3:15])=[CH2:3]

参加物

6

反応物 3

HCID 111,2-DichloroethaneHCID 65652,3-DichloropropeneHCID 7410Acetophenone

生成物 1

HCID 22404520HCID 22404520、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒2 回HCID 176Acetic Acid溶媒

実験手順

33.26 of 2,3-dichloro-1-propene were added dropwise to a mixture of 20.00 g of acetophenone, 40 g of ethylene dichloride, 60 g of 5% acetic acid and 19.52 g of zinc powder at 50° C., and the resultant mixture was allowed to react at the same temperature for 10 hours. After the reaction was completed, zinc-derived insolubles were filtered off, and the resultant filtrate was separated. The organic phase was washed with 7% sodium carbonate aqueous solution and dried over magnesium sulfate. The desiccant was filtered off, and the ethylene dichloride was distilled off under reduced pressure. The resultant oily substance was purified by silica gel column chromatography to give 22.24 g of 2-chloro-4-phenyl-1-penten-4-ol; nD25 =1.536, FI-MS m/e 178(M-H2O+), 180 (M-H2O+2+).

後処理

  1. customto react at the same temperature for 10 hours
  2. filtrationwere filtered off
  3. customthe resultant filtrate was separated
  4. washThe organic phase was washed with 7% sodium carbonate aqueous solution
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe desiccant was filtered off
  7. distillationthe ethylene dichloride was distilled off under reduced pressure
  8. customThe resultant oily substance was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bb7a193871524773bfe8c26031288bb6
出典データセット
uspto-grants-1996_06
特許番号
US05523495

反応ノート

読み込み中…