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

HRID 258725

反応式

HRID 258725 の反応式
[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]

参加物

5

反応物 4

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c195497bba66413cbd93778b6c8f84f3
出典データセット
uspto-grants-1977_07
特許番号
US04034108

関連ノート

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