HCID 86753081, 화합물 → HCID 18979156, 화합물

HRID 2393170노트

반응식

HRID 2393170 반응식
[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]

참가 물질

5

반응물 2

HCID 86753081HCID 86753081, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 18979156HCID 18979156, 화합물수율 129.1%

시약·촉매·용매 2

HCID 82844Platinum oxide (PtO)촉매HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-24db851d4a1a41d89b9b2ef0e6c68be7
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05804601

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