Diethyl Ether → Ethyl 5-(2-methoxyphenyl)-2-isoxazoline-3-carboxylate

HRID 1734977노트

반응식

HRID 1734977 반응식
F[C:2]1[CH:9]=[C:8](F)[CH:7]=[CH:6][C:3]=1[CH:4]=[CH2:5].Cl[C:12](=[N:18][OH:19])[C:13]([O:15][CH2:16][CH3:17])=[O:14].C[CH2:21][O:22]CC.C(N(CC)CC)C>O>[CH3:21][O:22][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]1[O:19][N:18]=[C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH2:5]1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 6816376Ethyl chloro(hydroximino)acetateHCID 202266752,4-Difluorostyrene

생성물 1

HCID 19436742Ethyl 5-(2-methoxyphenyl)-2-isoxazoline-3-carboxylate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

4.2 g of 2,4-difluorostyrene and 4.55 g of ethyl 2-chloro-2-hydroximinoacetate are introduced into 350 ml of ether, and the mixture is cooled to 0° C. 3.03 g of triethylamine are added dropwise to this mixture at 0° C. The mixture is stirred for 3 hours at room temperature, 50 ml of water are then added, and the mixture is extracted using ether. After drying over MgSO4, the ether is distilled off, and the residue is purified over a silica column (eluent: n-heptane:ethyl acetate=8:2). This gave 6.68 g (86% of theory) of product of refractive index [n]D20 =1.5019.

후처리

  1. extractionthe mixture is extracted
  2. dry with materialAfter drying over MgSO4
  3. distillationthe ether is distilled off
  4. customthe residue is purified over a silica column (eluent: n-heptane:ethyl acetate=8:2)

출처 및 근거

ORD 기록
ord-f7a72826af974f848273800ccd5b9792
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05536698

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