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

HRID 258339

반응식

HRID 258339 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 12375Ethylene glycol diethyl ether용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-33c268f57e78493faecfb13e5919d5f1
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266585

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