Water → 2-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane

HRID 351778

反応式

HRID 351778 の反応式
[C:1]1([CH3:7])C=CC=CC=1.O.[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]([C:18]2[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=2)=[O:17])=[CH:12][CH:11]=1.C1(C)C=CC(S(O)(=O)=[O:34])=CC=1>C(O)CO>[Cl:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]2([C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=3)[O:34][CH2:1][CH2:7][O:17]2)=[CH:14][CH:15]=1

参加物

6

反応物 4

HCID 962WaterHCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 3477714-Chloro-4'-nitrobenzophenone

生成物 1

HCID 154896262-(4-Chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane収率 91%

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

Toluene (1900 ml) was stirred in a round-bottom flask (5 l) using a water separator. (4-Chlorophenyl)(4-nitrophenyl)methanone (250 g) was added portionwise. p-Toluenesulfonic acid (54.5 g) was added portionwise. Ethylene glycol (237.5 g) was poured out into the mixture. The mixture was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was dissolved into ethyl acetate (5 l) and washed twice with a K2CO3 10% solution. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was stirred in DIPE, filtered off and dried (vacuum, 40° C., 24 hours), yielding 265 g (91%) of 2-(4-chlorophenyl)-2-(4-nitrophenyl)-1,3-dioxolane (interm. 5-a).

後処理

  1. temperaturerefluxed for 48 hours
  2. customThe solvent was evaporated
  3. dissolutionThe residue was dissolved into ethyl acetate (5 l)
  4. washwashed twice with a K2CO3 10% solution
  5. customThe organic layer was separated
  6. customdried
  7. filtrationfiltered
  8. customthe solvent was evaporated
  9. stirringThe residue was stirred in DIPE
  10. filtrationfiltered off
  11. customdried (vacuum, 40° C., 24 hours)

出典と根拠

ORDレコード
ord-70eac3638f2d4e448257f0b1645c5cf5
出典データセット
uspto-grants-2004_06
特許番号
US06743805B2

関連ノート

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