4,5-Dihydro-2,4,4-trimethyloxazole → 4,5-Dihydro-2-[2-(2-methoxy-5-nitrophenyl)ethenyl]-4,4-dimethyloxazole

HRID 621464

반응식

HRID 621464 반응식
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:4]=1[CH:5]=O.[CH3:14][C:15]1[O:16][CH2:17][C:18]([CH3:21])([CH3:20])[N:19]=1>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:4]=1[CH:5]=[CH:14][C:15]1[O:16][CH2:17][C:18]([CH3:21])([CH3:20])[N:19]=1

참가 물질

4

반응물 2

HCID 744964,5-Dihydro-2,4,4-trimethyloxazoleHCID 90685Benzaldehyde, 2-methoxy-5-nitro-

생성물 1

HCID 538942974,5-Dihydro-2-[2-(2-methoxy-5-nitrophenyl)ethenyl]-4,4-dimethyloxazole

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 2-methoxy-5-nitrobenzaldehyde, 16 g, (U.S. Pat. No. 4,367,234), 2,4,4-trimethyl-2-oxazoline, 30 ml, (Aldrich Chemical Company), para toluenesulfornic acid, 0.5 g, in toluene, 100 ml, is refluxed overnight under a water separator. The mixture is evaporated, the residue dissolved in diethylether, 800 ml, and washed with water. The diethyl ether layer is separated, concentrated, and filtered to give 11.1 g of 4,5-dihydro-2-[2-(2-methoxy-5-nitrophenyl)ethenyl]-4,4-dimethyloxazole after recrystallization from diisopropyl ether; mp 115°-116° C.

후처리

  1. customThe mixture is evaporated
  2. dissolutionthe residue dissolved in diethylether
  3. wash800 ml, and washed with water
  4. customThe diethyl ether layer is separated
  5. concentrationconcentrated
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-9a7318bef9cd4d248816b73663bb48a1
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824843

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