Triethylamine → HCID 178498980, 화합물

HRID 621422노트

반응식

HRID 621422 반응식
[NH2:1][C:2]([CH3:14])=[CH:3][C:4]([O:6][CH2:7][CH2:8][C:9]1[S:10][CH:11]=[CH:12][CH:13]=1)=[O:5].[N+:15]([C:18]1[CH:19]=[C:20]([CH:31]=[CH:32][CH:33]=1)[CH:21]=[C:22]([C:27](OC)=[O:28])[C:23]([O:25][CH3:26])=[O:24])([O-:17])=[O:16].C(N(CC)CC)C>CC(O)C>[OH:28][C:27]1[NH:1][C:2]([CH3:14])=[C:3]([C:4]([O:6][CH2:7][CH2:8][C:9]2[S:10][CH:11]=[CH:12][CH:13]=2)=[O:5])[CH:21]([C:20]2[CH:31]=[CH:32][CH:33]=[C:18]([N+:15]([O-:17])=[O:16])[CH:19]=2)[C:22]=1[C:23]([O:25][CH3:26])=[O:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 277557Dimethyl [(3-nitrophenyl)methylidene]propanedioateHCID 70042180HCID 70042180, 화합물

생성물 1

HCID 178498980HCID 178498980, 화합물수율 26.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 2-(2-thienyl)ethyl 3-amino-2-butenoate (1.8 g) and dimethyl 3-nitrobenzylidenemalonate (2.25 g) was dissolved in anhydrous 2-propanol (80 ml) and, after addition of triethylamine (27 ml), the mixture was refluxed for 21 hours. After the solvent was distilled off under reduced pressure, the residue was purified by thin-layer silica gel chromatography (developing solvent: chloroform/methanol=19/1; elution solvent: chloroform/acetone=2/1) so as to obtain 1.0 g (26%) of the desired compound.

후처리

  1. temperaturethe mixture was refluxed for 21 hours
  2. distillationAfter the solvent was distilled off under reduced pressure
  3. customthe residue was purified by thin-layer silica gel chromatography (developing solvent: chloroform/methanol=19/1; elution solvent: chloroform/acetone=2/1) so as

출처 및 근거

ORD 기록
ord-4787a4725a8343178e31938c9a9a0c99
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824837

반응 노트

불러오는 중…