2-(Ethylthio)ethanol → HCID 67937194, 화합물

HRID 652422

반응식

HRID 652422 반응식
[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]

참가 물질

6

반응물 3

HCID 80752-(Ethylthio)ethanolHCID 10868DicyclohexylcarbodiimideHCID 70048882HCID 70048882, 화합물

생성물 1

HCID 67937194HCID 67937194, 화합물수율 98%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 63651,1-Dichloroethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3354f2b148ac433c8f8a8d029cfaacb4
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04672068

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