2-(Ethylthio)ethanol → HCID 67937194、化合物

HRID 652422

反応式

HRID 652422 の反応式
[CH2:1]([O:10][C:11]([C:13]1[CH:18]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([N+:25]([O-:27])=[O:26])[CH:20]=2)[C:17]([C:28]([OH:30])=[O:29])=[C:16]([CH3:31])[NH:15][C:14]=1[CH3:32])=[O:12])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C1(N=C=NC2CCCCC2)CCCCC1.[CH2:48]([S:50][CH2:51][CH2:52]O)[CH3:49]>CN(C)C1C=CN=CC=1.ClC(Cl)C>[N+:25]([C:21]1[CH:20]=[C:19]([CH:18]2[C:17]([C:28]([O:30][CH2:49][CH2:48][S:50][CH2:51][CH3:52])=[O:29])=[C:16]([CH3:31])[NH:15][C:14]([CH3:32])=[C:13]2[C:11]([O:10][CH2:1][CH:2]=[CH:3][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)=[O:12])[CH:24]=[CH:23][CH:22]=1)([O-:27])=[O:26]

参加物

6

反応物 3

HCID 80752-(Ethylthio)ethanolHCID 10868DicyclohexylcarbodiimideHCID 70048882HCID 70048882、化合物

生成物 1

HCID 67937194HCID 67937194、化合物収率 98%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 63651,1-Dichloroethane溶媒

実験手順

434 mg (1 mM) of 4-(3-nitrophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylic acid monocinnamyl ester, 226 mg (1.1 mM) of dicyclohexylcarbodiimide, 122 mg (1 mM) of 4-dimethylaminopyridine and 127 mg (1.2 mM) of 2-ethylthioethanol were dissolved in 10 ml of dichloroethane, and refluxed for 2 hours. After the reaction mixture was chilled, insoluble matters were filtered off. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 511 mg of cinnamyl 2-ethylthioethyl 4-(3-nitrophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate (yield 98%).

後処理

  1. temperaturerefluxed for 2 hours
  2. temperatureAfter the reaction mixture was chilled
  3. filtrationinsoluble matters were filtered off
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-3354f2b148ac433c8f8a8d029cfaacb4
出典データセット
uspto-grants-1987_06
特許番号
US04672068

関連ノート

読み込み中…