Methanol → HCID 178471115, 화합물

HRID 657169노트

반응식

HRID 657169 반응식
[Na].[CH:2]([CH:4]([CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:5]([O:7]CC)=O)=O.[C:17]1(/[CH:23]=[CH:24]/[C:25](=[NH:27])[NH2:26])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.CO>CCO>[OH:7][C:5]1[C:4]([CH2:10][CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:2][N:27]=[C:25](/[CH:24]=[CH:23]/[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:26]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 14668188CinnamimidamideHCID 86635375Diethyl alpha-formylglutarate Sodium Salt

생성물 1

HCID 178471115HCID 178471115, 화합물수율 59.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Diethyl α-formylglutarate sodium salt (1 g, 4.2 mmol) and (2E)-3-phenyl-2-propenimidamide (0.61 g, 4.2 mmol), prepared in Example 126 (g), were combined in EtOH (20 mL) and MeOH (10 mL) and heated at reflux for 12 h. The solvent was removed and the resulting solid triturated with ether and filtered to give the desired product as a yellow solid (0.75 g, 56%). The mother liquor contained additional product which was not isolated. LCMS (ES+) m/z 299 (MH+).

후처리

  1. temperatureat reflux for 12 h
  2. customThe solvent was removed
  3. customthe resulting solid triturated with ether
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-acd65e24c48e471eae398574b5eef723
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071592B2

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