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

反応式

HRID 542774 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d3dcd6e82f24cff84d6d8aa644653d9
出典データセット
uspto-grants-1987_04
特許番号
US04659717

関連ノート

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