Diethyl (ethoxymethylene)malonate → HCID 178469787, 화합물

HRID 574659

반응식

HRID 574659 반응식
[Na].[CH2:2]([O:9][CH2:10][C:11]([NH2:13])=[NH:12])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([O:16][CH:17]=[C:18]([C:24](OCC)=O)[C:19]([O:21][CH2:22][CH3:23])=[O:20])C>CCO>[CH2:2]([O:9][CH2:10][C:11]1[N:13]=[C:17]([OH:16])[C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:24][N:12]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 6871Diethyl (ethoxymethylene)malonateHCID 4164062-PhenylmethoxyethanimidamideHCID 5360545Sodium

생성물 1

HCID 178469787HCID 178469787, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Sodium (4.6 g, 200 mmol) was added to EtOH (500 mL) and the mixture was stirred until a clear solution was obtained. Then, step B product, 2-c, (20.1 g, 100 mmol) and diethyl 2-(ethoxymethylene)malonate (21.6 g, 100 mmol) were added to the clear mixture, respectively. The reaction mixture was refluxed overnight and then concentrated under vacuum, washed with EA. The wet cake was then dried to afford compound 2-d (40.0 g, crude). LC-MS: (M+H)+ 289. The crude was directly used to next step without further purification.

후처리

  1. customwas obtained
  2. temperatureThe reaction mixture was refluxed overnight
  3. concentrationconcentrated under vacuum
  4. washwashed with EA
  5. customThe wet cake was then dried
  6. customto afford compound 2-d (40.0 g, crude)
  7. customThe crude was directly used to next step without further purification

출처 및 근거

ORD 기록
ord-941e7dbe208c45f5adc496c3dd093870
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034851B2

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