HCID 86753081、化合物 → HCID 18979156、化合物

HRID 2393170ノート

反応式

HRID 2393170 の反応式
[CH2:1]([O:3][C:4](=[O:22])[CH2:5][CH2:6][CH2:7][CH2:8][C:9](=[N:20]O)[C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=1)[CH3:2].NC(C1C=CC2C(=CC=CC=2)C=1)CCCCC(OCC)=O.[H][H]>C(O)(=O)C.[Pt]=O>[NH2:20][CH:9]([C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:11]=1)[CH2:8][CH2:7][CH2:6][CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:22]

参加物

5

反応物 2

HCID 86753081HCID 86753081、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 18979156HCID 18979156、化合物収率 129.1%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒HCID 176Acetic Acid溶媒

実験手順

Ethyl 6-amino-6-(2-naphthyl)hexanoate Ethyl 6-hydroxyimino-6-(2-naphthyl)hexanoate (19.2 g) and platinum oxide (0.96 g) were suspended in acetic acid (160 ml) and the suspension was stirred in a hydrogen atmosphere at room temperature for 10 hours. The catalyst was then filtered off and the filtrate was concentrated. The residue was dispersed in saturated aqueous sodium hydrogen carbonate solution and extracted with ethyl acetate. This extract was dried over anhydrous sodium sulfate and concentrated. The crude residue thus obtained was purified by silica gel column chromatography (ethyl acetate-methanol=10:1) to provide ethyl 6-amino-6-(2-naphthyl)hexanoate (12.1 g).

後処理

  1. filtrationThe catalyst was then filtered off
  2. concentrationthe filtrate was concentrated
  3. additionThe residue was dispersed in saturated aqueous sodium hydrogen carbonate solution
  4. extractionextracted with ethyl acetate
  5. dry with materialThis extract was dried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe crude residue thus obtained
  8. customwas purified by silica gel column chromatography (ethyl acetate-methanol=10:1)

出典と根拠

ORDレコード
ord-24db851d4a1a41d89b9b2ef0e6c68be7
出典データセット
uspto-grants-1998_09
特許番号
US05804601

反応ノート

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