Sulfuric Acid → N-(1,1-dimethyl-3-dimethylaminopropyl)acrylamide

HRID 267484노트

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HRID 267484 반응식
[C:1](#[N:4])[CH:2]=[CH2:3].S(=O)(=O)(O)O.[CH3:10][N:11]([CH3:17])[CH2:12][CH:13]=[C:14]([CH3:16])[CH3:15].C(C1C([OH:28])=C(C(C)(C)C)C=C(C)C=1)(C)(C)C.[OH-].[Na+]>O>[CH3:15][C:14]([NH:4][C:1](=[O:28])[CH:2]=[CH2:3])([CH3:16])[CH2:13][CH2:12][N:11]([CH3:17])[CH3:10]

참가 물질

7

반응물 5

HCID 1118Sulfuric AcidHCID 7855AcrylonitrileHCID 14798Sodium HydroxideHCID 314042,6-Di-tert-butyl-4-methylphenolHCID 52599752-Buten-1-amine, N,N,3-trimethyl-

생성물 1

HCID 1639462N-(1,1-dimethyl-3-dimethylaminopropyl)acrylamide

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

A resin flask is cooled to 0° C. and 450 grams (8.5 moles) of acrylonitrile, 1020 grams (10 moles) of sulfuric acid and 37 grams of water are added. To this mixture are then added 475 grams (4.2 moles) of the 1-dimethylamino-3-methyl-2-butene prepared as described above, and 8.5 grams of 2,6-di-t-butyl-p-cresol. The mixture is stirred at 68° C. for about 1 hour and is then neutralized with about 30% sodium hydroxide. The organic layer is separated, diluted with 2050 ml. of methanol and neutralized with ammonia. An additional 1000 ml. of methanol is added and the solution is filtered. The methanol is stripped from the filtrate and the residue is distilled. There is obtained 400 grams (64.5% of the theoretical amount) of the desired N-(1,1-dimethyl-3-dimethylaminopropyl)acrylamide boiling at 75°-92° C./0.25-0.9 mm. The nitrogen analysis is 15.4%, as compared with a theoretical value of 15.2%.

후처리

  1. customprepared
  2. customThe organic layer is separated
  3. additiondiluted with 2050 ml
  4. additionof methanol is added
  5. filtrationthe solution is filtered
  6. distillationthe residue is distilled

출처 및 근거

ORD 기록
ord-e12ee3a14c334806b57a51ab2aee0df8
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03943114

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