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

HRID 621464

反応式

HRID 621464 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9a7318bef9cd4d248816b73663bb48a1
出典データセット
uspto-grants-1989_04
特許番号
US04824843

関連ノート

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