4,5-Dihydro-2,4,4-trimethyloxazole → 5-(2'-Chloro-5'-nitrophenyl)-4-methyl-2,4-pentadienoic acid

HRID 893189

反応式

HRID 893189 の反応式
[OH:1]S([O-])=O.[Na+].[Cl:6][C:7]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][C:8]=1[CH:9]=[C:10]([CH3:13])[CH:11]=O.CC1[O:23][CH2:24][C:25](C)(C)N=1>C1(C)C=CC=CC=1>[Cl:6][C:7]1[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][C:8]=1[CH:9]=[C:10]([CH3:13])[CH:11]=[CH:25][C:24]([OH:1])=[O:23]

参加物

5

反応物 3

HCID 744964,5-Dihydro-2,4,4-trimethyloxazoleHCID 23665763Sodium BisulfiteHCID 544427022-Chloro-5-nitro-alpha-methylcinnamaldehyde

生成物 1

HCID 539242065-(2'-Chloro-5'-nitrophenyl)-4-methyl-2,4-pentadienoic acid

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

0.3 g of a 40 percent strength NaHSO3 solution is added to a mixture of 9 g of 2-chloro-5-nitro-α-methylcinnamaldehyde and 10.4 g of 2,4,4-trimethyloxazoline in 50 ml of toluene, and the mixture is refluxed for 10 hours. It is evaporated down, and 10 ml of water and 10 ml of concentrated HCl are added to the crude product of the structure ##STR23## Heating at 100° C. for 7 hours results in cleavage of the oxazoline ring. The crude product is filtered off under suction, washed with water and dried. Yield: 7.1 g (66%), mp. 178°-185° C.

後処理

  1. temperaturethe mixture is refluxed for 10 hours
  2. customIt is evaporated down
  3. addition10 ml of water and 10 ml of concentrated HCl are added to the crude product of the structure
  4. customresults in cleavage of the oxazoline ring
  5. filtrationThe crude product is filtered off under suction
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-1095fe112043484d9a4aa57594264db2
出典データセット
uspto-grants-1992_06
特許番号
US05123955

関連ノート

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