Triethylamine → Ethyl oxo-[N'-(3-phenylpropionyl)hydrazino]acetate

HRID 230789

反応式

HRID 230789 の反応式
[C:1]1([CH2:7][CH2:8][C:9]([NH:11][NH2:12])=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.Cl[C:21](=[O:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23]>C(Cl)(Cl)Cl>[O:27]=[C:21]([NH:12][NH:11][C:9](=[O:10])[CH2:8][CH2:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[C:22]([O:24][CH2:25][CH3:26])=[O:23]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 20884Ethoxalyl chlorideHCID 2493483-Phenylpropanehydrazide

生成物 1

HCID 68997631Ethyl oxo-[N'-(3-phenylpropionyl)hydrazino]acetate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

The 3-phenylpropionic acid hydrazide mixture (499 mg) obtained in Production Example 22-1 was dissolved in chloroform (30 mL), and triethylamine (0.86 mL) and ethyl chloroglyoxalate (0.4 mL) were added thereto, and stirred at room temperature for 5 hours. After the reaction, the reaction liquid was entirely concentrated, and the resulting residue was purified through silica gel column chromatography (chloroform/methanol=94/6) to obtain the entitled compound (760 mg).

後処理

  1. customAfter the reaction
  2. customthe reaction liquid
  3. concentrationwas entirely concentrated
  4. customthe resulting residue was purified through silica gel column chromatography (chloroform/methanol=94/6)

出典と根拠

ORDレコード
ord-6feddf2aa9af48918ff794a2e92064c8
出典データセット
uspto-grants-2009_07
特許番号
US07566781B2

関連ノート

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