Methanesulfonyl chloride → HCID 18979131, 화합물

HRID 2393181노트

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HRID 2393181 반응식
[NH2:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]([O:20]COC)=[O:19].[S:24](Cl)([CH3:27])(=[O:26])=[O:25]>N1C=CC=CC=1.Cl>[S:24]([NH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:20])=[O:19])([CH3:27])(=[O:26])=[O:25]

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 18979130HCID 18979130, 화합물

생성물 1

HCID 18979131HCID 18979131, 화합물수율 84.5%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 1049Pyridine용매

반응 조건

온도
50 °C

실험 절차

In pyridine (3 ml) was dissolved methoxymethyl 7-(1-amino-2-naphthyl)heptanoate (0.3 g) followed by addition of mesyl chloride (0.218 g), and the mixture was stirred at 50° C. for 2 hours. This reaction mixture was poured in 0.5N HCl and extracted with ethyl acetate. The organic layer was washed with water, dried, and concentrated to dryness. The residue was treated with 1N HCl (3 ml) and tetrahydrofuran (6 ml) at the reflux temperature for 1.5 hours and, after cooling, extracted with ethyl acetate. The organic layer was washed with water, dried, and concentrated to dryness, and the residue was recrystallized from hexane-diisopropyl ether to provide 7-(1-mesylamino-2-naphthyl)heptanoic acid (0.281 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated to dryness
  5. additionThe residue was treated with 1N HCl (3 ml) and tetrahydrofuran (6 ml) at the reflux temperature for 1.5 hours
  6. temperatureafter cooling
  7. extractionextracted with ethyl acetate
  8. washThe organic layer was washed with water
  9. customdried
  10. concentrationconcentrated to dryness
  11. customthe residue was recrystallized from hexane-diisopropyl ether

출처 및 근거

ORD 기록
ord-f400a2d39b82438bad1c1cea4f6c967a
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05804601

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