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Aniline → N-benzene sulfonyl phenyl cyanamide

HRID 26391
ノート
印刷プレビュー

反応式

HRID 26391 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1N2C[CH2:15][N:10](CC2)C1.[C:16]1([S:22](Cl)(=[O:24])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.N#CCl>C1COCC1>[C:16]1([S:22]([N:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:15]#[N:10])(=[O:24])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6115AnilineHCID 7369Benzenesulfonyl chlorideHCID 9237DabcoHCID 10477Cyanogen Chloride

生成物 1

HCID 21323003N-benzene sulfonyl phenyl cyanamide収率 84.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a 3 liter 3-necked flask equipped with a stirrer, addition funnel, thermometer, and drying tube was charged 93.1 g (1.0 mole) of aniline, 111 g (1.1 moles) of triethylene diamine and 250 ml. of tetrahydrofuran. To this reaction mixture was added dropwise a solution of 176.6 g (1 mole) of benzenesulfonyl chloride in 300 ml. of tetrahydrofuran. The reaction mixture was stirred at room temperature for 2.5 hours and was then filtered. To the filtrate was added 111 g of triethylene diamine and this solution was added dropwise to a solution of 87 g (1.41 moles) of cyanogen chloride in 100 ml. of THF which was maintained at -5° C. with cooling. After this addition was complete the stirred reaction mixture was allowed to return to room temperature over a 161/2 hour period. The reaction mixture was filtered and the filament was added to water to precipitate the product. The product was recrystallized from aqueous methanol to yield 218 g (84.7%) of N-benzene sulfonyl phenyl cyanamide, m.p. 65°-66° C.

後処理

  1. customTo a 3 liter 3-necked flask equipped with a stirrer, addition funnel
  2. customthermometer, and drying tube
  3. filtrationwas then filtered
  4. additionTo the filtrate was added 111 g of triethylene diamine
  5. temperaturewith cooling
  6. additionAfter this addition
  7. customthe stirred reaction mixture
  8. customto return to room temperature over a 161
  9. custom2 hour period
  10. filtrationThe reaction mixture was filtered
  11. additionthe filament was added to water
  12. customto precipitate the product
  13. customThe product was recrystallized from aqueous methanol

出典と根拠

ORDレコード
ord-93251148a7124554a88961efd1b18c6f
出典データセット
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04150051

反応ノート

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