Carbon Dioxide → 2-[p-(Phenoxy)-phenyl]-2-[1-(1H-1,2,4-triazolyl)-methyl]-1,3-dioxolane

HRID 258339

反応式

HRID 258339 の反応式
O([C:8]([O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2([CH2:22][N:23]3[CH:27]=[N:26][CH:25]=[N:24]3)[O:21][CH2:20][CH2:19][O:18]2)=[CH:13][CH:12]=1)=O)C1C=CC=CC=1.C(=O)=O>C(OCCOCC)C.C(OCC)C>[O:10]([C:11]1[CH:12]=[CH:13][C:14]([C:17]2([CH2:22][N:23]3[CH:27]=[N:26][CH:25]=[N:24]3)[O:18][CH2:19][CH2:20][O:21]2)=[CH:15][CH:16]=1)[C:8]1[CH:15]=[CH:16][CH:11]=[CH:12][CH:13]=1

参加物

5

反応物 2

HCID 280Carbon DioxideHCID 197374212-[p-(Phenoxycarbonyloxy)-phenyl]-2-[1-(1H-1,2,4-triazolyl)-methyl]-1,3-dioxolane

生成物 1

HCID 197373892-[p-(Phenoxy)-phenyl]-2-[1-(1H-1,2,4-triazolyl)-methyl]-1,3-dioxolane

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 12375Ethylene glycol diethyl ether溶媒

実験手順

11 parts of 2-[p-(Phenoxycarbonyloxy)-phenyl]-2-[1-(1H-1,2,4-triazolyl)-methyl]-1,3 -dioxolane are heated in 200 ml ethylene glycol diethyl ether (about 10 hours) at a temperature of 130° C. till the end of the carbon dioxid production. Then the solvent is destilled of under reduced pressure. The oily crude product is cooled to room temperature, solved in 500 ml diethyl ether, washed with two portions of 100 ml water, dried over sodium sulfate and filtered. The solvent is removed by evaporation. The crude product is recrystallised from ethyl acetate/cyclohexane in the presence of active carbon to give colourless crystals with a melting point of 100°-102° C.

後処理

  1. washwashed with two portions of 100 ml water
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. customThe solvent is removed by evaporation
  5. customThe crude product is recrystallised from ethyl acetate/cyclohexane in the presence of active carbon
  6. customto give colourless crystals with a melting point of 100°-102° C.

出典と根拠

ORDレコード
ord-33c268f57e78493faecfb13e5919d5f1
出典データセット
uspto-grants-1993_11
特許番号
US05266585

関連ノート

読み込み中…