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Carbon Dioxide → N-(1,1-dimethyl-3-dimethylaminobutyl)acrylamide

HRID 1576141
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HRID 1576141 반응식
[CH3:1][C:2]([NH:10][C:11](=[O:16])[CH2:12][CH2:13]OC)([CH3:9])[CH2:3][CH:4]([N:6]([CH3:8])[CH3:7])[CH3:5].[OH-].[Na+].C1(C=CC(O)=CC=1)O.C(=O)=O>>[CH3:9][C:2]([NH:10][C:11](=[O:16])[CH:12]=[CH2:13])([CH3:1])[CH2:3][CH:4]([N:6]([CH3:8])[CH3:7])[CH3:5]
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참가 물질

5

반응물 4

HCID 280Carbon DioxideHCID 785HydroquinoneHCID 14798Sodium HydroxideHCID 21514639HCID 21514639, 화합물

생성물 1

HCID 20432749N-(1,1-dimethyl-3-dimethylaminobutyl)acrylamide

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온도
80 °C

실험 절차

A mixture of 144.7 parts (0.63 mole) of N-(1,1-dimethyl-3-dimethylaminobutyl)-3-methoxypropionamide, 1 part of solid sodium hydroxide and 1 part of hydroquinone is charged to a reaction flask fitted with a condenser with a Dry Ice-cooled receiver, a stirrer and temperature control means. The pressure in the flask is reduced to less than 5 mm. and the flask is heated to 80°C. Vigorous reaction begins and liquid condenses in the receiver. After about one-half hour, the temperature is increased to 90°C. and this temperature is maintained for 3 hours. The product is distilled and the desired N-(1,1-dimethyl-3-dimethylaminobutyl)acrylamide is obtained at 80°-91°C./ 0.3-0.4 mm. The yield is 109.1 parts, or 87.4% of the theoretical amount, and the nitrogen percentage is the calculated 14.1%.

후처리

  1. additionis charged to a reaction flask
  2. temperaturecooled receiver, a stirrer and temperature control
  3. customVigorous reaction
  4. waitAfter about one-half hour
  5. temperaturethe temperature is increased to 90°C.
  6. temperaturethis temperature is maintained for 3 hours
  7. distillationThe product is distilled

출처 및 근거

ORD 기록
ord-b19454035b3e4d71a4c9a39961d346dd
출처 데이터셋
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03979441

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