Diisopropylethylamine → ethyl (E)-3-[(E)-aminomethylideneamino]-2-cyano-3-[(4-methoxyphenyl)methylamino]prop-2-enoate

HRID 1052386노트

반응식

HRID 1052386 반응식
[C:1](/[C:3](=[C:9](/[NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)\SC)/[C:4]([O:6][CH2:7][CH3:8])=[O:5])#[N:2].C(N(CC)C(C)C)(C)C.Cl.[CH:32]([NH2:34])=[NH:33]>C(O)C>[NH2:34]/[CH:32]=[N:33]/[C:9](/[NH:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)=[C:3](\[C:1]#[N:2])/[C:4]([O:6][CH2:7][CH3:8])=[O:5]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 10313058Methanimidamide, hydrochloride (1:1)HCID 131736126(E)-Ethyl 2-cyano-3-((4-methoxybenzyl)amino)-3-(methylthio)acrylate

생성물 1

HCID 140693035ethyl (E)-3-[(E)-aminomethylideneamino]-2-cyano-3-[(4-methoxyphenyl)methylamino]prop-2-enoate수율 25%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(E)-Ethyl 2-cyano-3-((4-methoxybenzyl)amino)-3-(methylthio)acrylate was dissolved in 65 mL ethanol. N,N-Diisopropylethylamine (13 mL, 74.44 mmol) and formamidine hydrochloride (2.12 g, 26.33 mmol) were added and the reaction mixture was stirred at room temperature for 48 h. The solvent was concentrated and the residue was directly purified using SP1® Purification System (0% to 10%, dichloromethane-methanol) to give 0.96 g (25% yield) of the title compound as a yellow oil. Purity 85%.

후처리

  1. concentrationThe solvent was concentrated
  2. customthe residue was directly purified
  3. customSP1® Purification System (0% to 10%, dichloromethane-methanol)

출처 및 근거

ORD 기록
ord-481c52aaed3041dab195f422e109fc60
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388189B2

반응 노트

불러오는 중…