Pyridine → Sulfamic acid 2-(methoxycarbonyl)propyl ester

HRID 1613442노트

반응식

HRID 1613442 반응식
[C:1]([O-:5])(=[O:4])CC.[S:6](=[O:16])(=[O:15])([O:8]C1C=CC=CC=1)[NH2:7].[C:17]1(C)C=CC=CC=1.N1[CH:29]=[CH:28][CH:27]=CC=1>>[CH3:17][O:5][C:1]([CH:28]([CH3:27])[CH2:29][O:16][S:6](=[O:15])(=[O:8])[NH2:7])=[O:4]

참가 물질

5

반응물 4

HCID 1049PyridineHCID 1140TolueneHCID 104745Propionate ionHCID 11030308Phenylsulfamate

생성물 1

HCID 54337150Sulfamic acid 2-(methoxycarbonyl)propyl ester수율 40%

실험 절차

A mixture of 5.9 g (0.05 mole) of (S)-(+)methyl 3-hydroxy-2-methyl]propionate, 9.5 g (0.055 mole) of phenyl sulfamate, 25 ml of toluene and 0.5 g of pyridine was heated at reflux for 2 hr. The reaction solution was concentrated under vacuum, and the residue was chromatographed, using silica gel and eluting with 2% methanol in methylene chloride. The desired fractions were concentrated under vacuum to give 3.9 g (40%) of a pale yellow oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 hr
  3. concentrationThe reaction solution was concentrated under vacuum
  4. customthe residue was chromatographed
  5. washeluting with 2% methanol in methylene chloride
  6. concentrationThe desired fractions were concentrated under vacuum

출처 및 근거

ORD 기록
ord-360d6c408be7498baf02059a85ef92bf
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05192785

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