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Dabco → HCID 68140610、化合物

HRID 267592
ノート
印刷プレビュー

反応式

HRID 267592 の反応式
[C:1]1([CH3:10])[CH:6]=[CH:5][C:4]([S:7](Cl)=[O:8])=[CH:3][CH:2]=1.[NH2:11][C:12]1[CH:17]=[CH:16][C:15]([S:18]([CH:21]=[CH:22][C:23]#[N:24])(=[O:20])=[O:19])=[CH:14][CH:13]=1.N12CCN(CC1)CC2>CC(C)=O>[CH3:10][C:1]1[CH:6]=[CH:5][C:4]([S:7]([NH:11][C:12]2[CH:13]=[CH:14][C:15]([S:18]([CH:21]=[CH:22][C:23]#[N:24])(=[O:20])=[O:19])=[CH:16][CH:17]=2)=[O:8])=[CH:3][CH:2]=1
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 9237DabcoHCID 41900044-Methylbenzene-1-sulfinyl chlorideHCID 545613262-Cyanovinyl 4-aminophenyl sulfone

生成物 1

HCID 68140610HCID 68140610、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒3 回

実験手順

17.5 g p-toluenesulfinyl chloride (obtained by treating sodium toluenesulfinate.2H2O with thionyl chloride) is dissolved in 100 ml of acetone and this solution is added at room temperature and with stirring to a solution of 20.8 g (0.1 mol) of 2-cyanovinyl 4-aminophenyl sulfone in 250 ml of acetone. Shortly thereafter a solution of 11.2 g (0.1 mol) of 1,4-diazabicyclo[2.2.2]octane in 150 ml of acetone is added over about 10 minutes and the reaction mixture is stirred for another 20 minutes. The reaction mixture is filtered, evaporated in air to about a third of its volume, and then poured into cold water. The precipitate is filtered, washed and dried to give 3-[4-(4-methylbenzenesulfinamido)benzenesulfonyl]acrylonitrile: ##SPC45##

後処理

  1. additionthis solution is added at room temperature
  2. filtrationThe reaction mixture is filtered
  3. customevaporated in air to about a third of its volume
  4. additionpoured into cold water
  5. filtrationThe precipitate is filtered
  6. washwashed
  7. customdried

出典と根拠

ORDレコード
ord-47a1697a1e5648b68c6e652a38023d48
出典データセット
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03943154

反応ノート

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