2-Butenoic acid, 3-amino-, ethyl ester, (2Z)- → 1,4-Dihydro-2,6-dimethyl-4-(2-methylbenzo[b]thien-3-yl)-3,5-pyridinedicarboxylic acid, diethyl ester

HRID 542774

반응식

HRID 542774 반응식
[CH3:1][C:2]1[S:6][C:5]2[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=2[C:3]=1[CH:11]=O.[NH2:13]/[C:14](/[CH3:21])=[CH:15]\[C:16]([O:18][CH2:19][CH3:20])=[O:17]>C(O)C>[CH3:21][C:14]1[NH:13][C:14]([CH3:21])=[C:15]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:11]([C:3]2[C:4]3[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=3[S:6][C:2]=2[CH3:1])[C:15]=1[C:16]([O:18][CH2:19][CH3:20])=[O:17]

참가 물질

4

반응물 2

HCID 6437562-Butenoic acid, 3-amino-, ethyl ester, (2Z)-2회HCID 37754672-Methyl-1-benzothiophene-3-carbaldehyde

생성물 1

HCID 138268541,4-Dihydro-2,6-dimethyl-4-(2-methylbenzo[b]thien-3-yl)-3,5-pyridinedicarboxylic acid, diethyl ester수율 43.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2.2 g of 2-methylbenzo[b]thiophene-3-carboxaldehyde, 4.9 g of ethyl 3-aminocrotonate, and 10 ml of ethanol were heated to reflux for approximately 18 hours. An additional 1.6 g of ethyl 3-aminocrotonate were added and the reaction was heated an additional 24 hours at reflux. The reaction mixture was cooled and concentrated and the resulting solid was recovered by filtration providing 2.15 g of the desired title product, m.p. 191°-193° C.

후처리

  1. temperaturewere heated
  2. temperatureto reflux for approximately 18 hours
  3. temperaturethe reaction was heated an additional 24 hours
  4. temperatureat reflux
  5. temperatureThe reaction mixture was cooled
  6. concentrationconcentrated
  7. filtrationthe resulting solid was recovered by filtration

출처 및 근거

ORD 기록
ord-1d3dcd6e82f24cff84d6d8aa644653d9
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659717

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