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Chlorosulfonic acid → 4-(2-Oxoimidazolidin-1-yl)benzenesulfonyl chloride

HRID 746747
ノート
印刷プレビュー

反応式

HRID 746747 の反応式
[Cl:1][S:2]([OH:5])(=O)=[O:3].C([N:13]1[CH2:17][CH2:16][N:15]([C:18]2[CH:23]=[CH:22][C:21](S(NC3C=CC=CC=3C(C3C=CC(F)=CN=3)=O)(=O)=O)=[CH:20][CH:19]=2)[C:14]1=[O:43])C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[O:43]=[C:14]1[NH:13][CH2:17][CH2:16][N:15]1[C:18]1[CH:23]=[CH:22][C:21]([S:2]([Cl:1])(=[O:5])=[O:3])=[CH:20][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 58664909HCID 58664909、化合物

生成物 1

HCID 214290354-(2-Oxoimidazolidin-1-yl)benzenesulfonyl chloride

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

To 1.5 mL (23.1 mmol) of chlorosulfonic acid in 3 mL of carbon tetrachloride at 0° C. was added slowly 500 mg (3.1 mmol) of the compound of Step 1. The reaction was almost completed after 2 h at 0° C. The reaction mixture was poured into ice water slowly, then filtered to collect the solids formed. The aqueous layer was extracted with chloroform (3×100 ml), and the combined organic layers were dried over sodium sulfate, filtered, concentrated in vacuo. The filtered solid and the crude material from the extraction were combined to provide the title compound (LC/MS found: 261.1)

後処理

  1. filtrationfiltered
  2. customto collect the solids
  3. customformed
  4. extractionThe aqueous layer was extracted with chloroform (3×100 ml)
  5. dry with materialthe combined organic layers were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. extractionThe filtered solid and the crude material from the extraction

出典と根拠

ORDレコード
ord-e4065a2568f149a8887165f4b43e54db
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07393873B2

反応ノート

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