Carbon Dioxide → Methyl N-(2,6-dimethylphenyl)-DL-alaninate

HRID 258725

반응식

HRID 258725 반응식
[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:3]=1[NH2:4].C([O-])(O)=O.[Na+].[CH3:15][O:16][C:17](=[O:21])[CH:18](Br)[CH3:19].C(=O)=O>>[CH3:15][O:16][C:17](=[O:21])[CH:18]([NH:4][C:3]1[C:5]([CH3:9])=[CH:6][CH:7]=[CH:8][C:2]=1[CH3:1])[CH3:19]

참가 물질

5

반응물 4

HCID 280Carbon DioxideHCID 68962,6-DimethylanilineHCID 95576Methyl 2-bromopropionateHCID 516892Sodium Bicarbonate

생성물 1

HCID 94555Methyl N-(2,6-dimethylphenyl)-DL-alaninate

실험 절차

6 g-moles of 2,6-dimethylaniline, 6.6 g-moles of NaHCO3 and 18.0 g-moles of α-bromopropionic acid methyl ester are placed together and heated slowly, with stirring, for 1 hour upto 120°-125° C. bath temperature. As CO2 is evolved, stirring of the mixture at this temperature is continued for 18 hours. The mixture is subsequently cooled, the inorganic constituents are filtered off, and the filtrate distilled in a water-jet vacuum (ca. 10- 12 Torr). After removal of the excess α-bromopropionic acid methyl ester, the resulting yield is 990.3 g (79.6% of theory) of final product, which boils at 133°-134° (12 Torr).

후처리

  1. temperatureheated slowly
  2. stirringstirring of the mixture at this temperature
  3. waitis continued for 18 hours
  4. temperatureThe mixture is subsequently cooled
  5. filtrationthe inorganic constituents are filtered off
  6. distillationthe filtrate distilled in a water-jet vacuum (ca. 10- 12 Torr)
  7. customAfter removal of the excess α-bromopropionic acid methyl ester

출처 및 근거

ORD 기록
ord-c195497bba66413cbd93778b6c8f84f3
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04034108

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