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

HRID 893189

반응식

HRID 893189 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1095fe112043484d9a4aa57594264db2
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05123955

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