Water → HCID 54100550, 화합물

HRID 1595501

반응식

HRID 1595501 반응식
[CH:1]([C:3]1[CH:25]=[CH:24][C:6]([O:7][CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:23])[O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[CH:12][CH:11]=2)=[CH:5][CH:4]=1)=O.[S:26]1[CH2:30][C:29](=[O:31])[NH:28][C:27]1=[O:32].C([O-])(=O)C.[NH2+]1CCCCC1.O>C1(C)C=CC=CC=1>[C:19]([O:18][C:17]([NH:16][C:13]1[CH:12]=[CH:11][C:10]([CH2:9][CH2:8][O:7][C:6]2[CH:5]=[CH:4][C:3]([CH:1]=[C:30]3[S:26][C:27](=[O:32])[NH:28][C:29]3=[O:31])=[CH:25][CH:24]=2)=[CH:15][CH:14]=1)=[O:23])([CH3:22])([CH3:20])[CH3:21]

참가 물질

6

반응물 4

HCID 962WaterHCID 5437Thiazolidinedione2회HCID 3014295Piperidinium acetateHCID 21704970tert-butyl N-{4-[2-(4-formylphenoxy)ethyl]phenyl}carbamate

생성물 1

HCID 54100550HCID 54100550, 화합물수율 72.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 3.41 g (10 mmole) tert-butyl N-{4-[2-(4-formylphenoxy)ethyl]phenyl}carbamate and 1.29 g (11 mmole) 2,4-thiazolidinedione in toluene containing a catalytic amount of piperidinium acetate was refluxed in a Dean-Stark water trap for 3 hours. The reaction was followed by TLC and more 2,4-thiazolidinedione was added during the reaction time. The solution was cooled to room temperature filtered and the precipitate was refluxed in methanol. Another filtration gave 3.2 g (yield 72.6%) 5-(4-[2-(4-tert-butyloxycarbonylaminophenyl)ethoxy]benzylidene)thiazolidine-2,4-dione as a light yellow, solid substance.

후처리

  1. additionwas added during the reaction time
  2. filtrationfiltered
  3. temperaturethe precipitate was refluxed in methanol
  4. filtrationAnother filtration

출처 및 근거

ORD 기록
ord-d4ad7562dded438cb015b98b0f89d2f4
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288096B1

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