Methanesulfonyl chloride → 3-(4-Methanesulfonamidobenzenesulfonyl)acrylonitrile

HRID 267576ノート

反応式

HRID 267576 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:12]=[CH:11][C:10]([S:13]([CH:16]=[CH:17][C:18]#[N:19])(=[O:15])=[O:14])=[CH:9][CH:8]=1>C(Cl)(Cl)Cl.N1C=CC=CC=1>[CH3:1][S:2]([NH:6][C:7]1[CH:8]=[CH:9][C:10]([S:13]([CH:16]=[CH:17][C:18]#[N:19])(=[O:15])=[O:14])=[CH:11][CH:12]=1)(=[O:4])=[O:3]

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 545613262-Cyanovinyl 4-aminophenyl sulfone

生成物 1

HCID 545373813-(4-Methanesulfonamidobenzenesulfonyl)acrylonitrile

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒2 回HCID 6212Chloroform溶媒

実験手順

23 grams (0.2 mol) of methanesulfonyl chloride (CH3SO2Cl) are dissolved in 600 milliliters of chloroform, and 42 grams (0.2 mol) of 3-(4-aminobenzenesufonyl)acrylonitrile, prepared as described in copending application Ser. No. 228,410 filed Feb. 22, 1972, are added with stirring and cooling in an ice bath followed portionwise by a solution of 16 g (0.2 mol) of pyridine in 200 ml of pyridine. The reaction mixture is allowed to reach room temperature and is thereafter left at about 20° C for about 48 hours. The solution is filtered and then washed with water, a 5% solution of HCl in water, a 5% sodium bicarbonate solution in water, and water, in sequence.

後処理

  1. addition22, 1972, are added
  2. temperaturecooling in an ice bath
  3. customto reach room temperature
  4. filtrationThe solution is filtered
  5. washwashed with water

出典と根拠

ORDレコード
ord-54d081fb94394428a82071b0204d67a2
出典データセット
uspto-grants-1976_03
特許番号
US03943154

反応ノート

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