Formaldehyde → HCID 53746566、化合物

HRID 1934571ノート

反応式

HRID 1934571 の反応式
C=O.[O:3]=[C:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]([C:13]([OH:15])=[O:14])[CH2:5]1.N1CCCC[CH2:17]1.[CH3:22][O:23][C:24](=[O:32])[C@H:25]([CH2:30][SH:31])[NH:26][C:27](=[O:29])[CH3:28]>C(O)C>[C:27]([NH:26][C@H:25]([C:24]([O:23][CH3:22])=[O:32])[CH2:30][S:31][CH2:17][CH:5]1[C:4](=[O:3])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]1[C:13]([OH:15])=[O:14])(=[O:29])[CH3:28]

参加物

6

反応物 4

HCID 712FormaldehydeHCID 8082PiperidineHCID 998151H-Indene-1-carboxylic acid, 2,3-dihydro-3-oxo-HCID 6542158L-Cysteine, N-acetyl-, methyl ester

生成物 1

HCID 53746566HCID 53746566、化合物収率 37.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

After 37% formalin (0.088 ml, 1.08 mmol) was added to a mixture of 3-oxo-1-indanecarboxylic acid (191 mg, 1.08 mmol) and piperidine (92.3 mg, 1.08 mmol), the mixture was stirred at room temperature for 3 hours. The reaction solution was concentrated. Ethanol (3 ml) and N-acetyl-L-cysteine methyl ester (80 mg, 0.45 mmol) were added to the residue. The mixture was heated to reflux for 10 minutes and then concentrated in vacuo. The residue was purified by silica gel column chromatography (100 ml, chloroform:methanol:acetic acid=30:1:0.5) to give Compound (6A) (62 mg, yield: 15.7%).

後処理

  1. concentrationThe reaction solution was concentrated
  2. temperatureThe mixture was heated
  3. temperatureto reflux for 10 minutes
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by silica gel column chromatography (100 ml, chloroform:methanol:acetic acid=30:1:0.5)

出典と根拠

ORDレコード
ord-b8c4222dff4f4359b2551b9bcea2f8d1
出典データセット
uspto-grants-2002_05
特許番号
US06384063B1

反応ノート

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