Methanol → HCID 178471115、化合物

HRID 657169ノート

反応式

HRID 657169 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178471115HCID 178471115、化合物収率 59.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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+).

後処理

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

出典と根拠

ORDレコード
ord-acd65e24c48e471eae398574b5eef723
出典データセット
uspto-grants-2011_12
特許番号
US08071592B2

反応ノート

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