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Acrylic Acid → HCID 86738178、化合物

HRID 1660302
ノート
印刷プレビュー

反応式

HRID 1660302 の反応式
[CH2:1]([N:4]([CH2:13][CH:14]=[CH2:15])[CH:5]=[CH:6][CH:7]=[C:8]([C:11]#[N:12])[C:9]#[N:10])[CH:2]=[CH2:3].[C:16]([OH:20])(=[O:19])[CH:17]=[CH2:18].C(OOC(=O)CCCCCCCCCCC)(=O)CCCCCCCCCCC>C(O)C>[C:16]([OH:20])(=[O:19])[CH:17]=[CH2:18].[CH2:1]([N:4]([CH:5]=[CH:6][CH:7]=[C:8]([C:9]#[N:10])[C:11]#[N:12])[CH2:13][CH:14]=[CH2:15])[CH:2]=[CH2:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6581Acrylic Acid5 回HCID 7773Lauroyl peroxide5 回HCID 53724731{3-[Di(prop-2-en-1-yl)amino]prop-2-en-1-ylidene}propanedinitrile

生成物 1

HCID 86738178HCID 86738178、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒5 回

実験手順

60 g. of intermediate (A) and 20 g. of acrylic acid were diluted in 120 cc. of ethanol in a flask with stirrer and reflux and 2 g. of lauroyl peroxide were added, and then reflux heated. After one hour, 16 g. of acrylic acid and 1 g. of lauroyl peroxide diluted in 20 g. of ethanol were added; always continuing the reflux heating, at one hour time intervals the following additions were made: 13 g. of acrylic acid and 1 g. of lauroyl peroxide in 20 cc. of ethanol; 10 g. of acrylic acid and 0.8 g. of lauroyl peroxide in 15 cc. of ethanol; 8 g. of acrylic acid and 0.8 g. of lauroyl peroxide in 10 cc. of ethanol. After the last addition the mixture was refluxed for two hours, then it was cooled, and precipitated in ethyl ether; the precipitate was recovered on filter, washed with ether and vacuum dried at 50° C. The yield was 49 g. of a product containing about 23% of aminoallylidenemalononitrile units. The product was water and NaOH at pH=7 soluble. A solution at 6% 1:9000 diluted with water, had an optical density of 0.46.

後処理

  1. temperaturereflux
  2. temperatureheated
  3. temperatureheating, at one hour time intervals the following additions
  4. additionAfter the last addition the mixture
  5. temperaturewas refluxed for two hours
  6. temperatureit was cooled
  7. customprecipitated in ethyl ether
  8. customthe precipitate was recovered
  9. filtrationon filter
  10. washwashed with ether and vacuum
  11. customdried at 50° C
  12. additionof a product containing about 23% of aminoallylidenemalononitrile units
  13. additionA solution at 6% 1:9000 diluted with water

出典と根拠

ORDレコード
ord-a0b8294ef8bb4614a6514ded73313b26
出典データセット
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04307184

反応ノート

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