1H-1,2,4-Triazole → Ethyl 6-[p-[5-(1,2,4-triazol-1-yl)pentyloxy]phenoxy]-2,2-dimethylhexanoate

HRID 329467노트

반응식

HRID 329467 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:26]=[CH:25][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([CH3:24])([CH3:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:10][CH:9]=1.[Na].[NH:28]1[CH:32]=[N:31][CH:30]=[N:29]1>CN(C=O)C>[N:28]1([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]2[CH:26]=[CH:25][C:11]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([CH3:24])([CH3:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:10][CH:9]=2)[CH:32]=[N:31][CH:30]=[N:29]1

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 5360545SodiumHCID 14851566Ethyl 6-[p-(5-bromopentyloxy)phenoxy]-2,2-dimethylhexanoate

생성물 1

HCID 14327307Ethyl 6-[p-[5-(1,2,4-triazol-1-yl)pentyloxy]phenoxy]-2,2-dimethylhexanoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2.16 g ethyl 6-[p-(5-bromopentyloxy]phenoxy)-2,2-dimethylhexanoate in 10 ml DMF, was added with stirring 0.55 g sodium salt of 1,2,4-triazole at room temperature, and stirring was continued overnight. DMF was distilled off under reduced pressure, the residue was extracted with chloroform, and the extract was washed with water, dried and concentrated. The crude product thus obtained was purified by silica gel column chromatography, affording 1.21 g of ethyl 6-[p-[5-(1,2,4-triazol-1-yl)pentyloxy]phenoxy]-2,2-dimethylhexanoate.

후처리

  1. distillationDMF was distilled off under reduced pressure
  2. extractionthe residue was extracted with chloroform
  3. washthe extract was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe crude product thus obtained
  7. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-b822d86399a74df8b5387cc9d1022eb9
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04891432

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