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Iodine chloride → 1-(4-Amino-3-iodophenyl)-N-methylmethanesulfonamide

HRID 1647770
ノート
印刷プレビュー

反応式

HRID 1647770 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][S:9]([NH:12][CH3:13])(=[O:11])=[O:10])=[CH:4][CH:3]=1.[I:14]Cl>C(#N)C>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][S:9]([NH:12][CH3:13])(=[O:11])=[O:10])=[CH:4][C:3]=1[I:14]
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 24640Iodine chlorideHCID 27781314-Amino-N-methylbenzenemethanesulfonamide

生成物 1

HCID 107584621-(4-Amino-3-iodophenyl)-N-methylmethanesulfonamide収率 65.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 1.06 g (5.31 mmol, 1.0 equiv.) of 4-amino-N-methylbenzenemethanesulfonamide in 20 mL of acetonitrile was added 0.862 g (5.31 mmol, 1.0 equiv.) of iodine monochloride. The reaction was stirred for 15 minutes at room temperature. The mixture was partitioned between 25 mL of ethyl acetate and 15 mL of 20% aqueous sodium thiosulfate. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to yield an oil. The oil was filtered through a plug of silica gel using 40% ethyl acetate in hexane to yield 1.13 g (65%) of 4-amino-3-iodo-N-methylbenzenemethanesulfonamide.

後処理

  1. customThe mixture was partitioned between 25 mL of ethyl acetate and 15 mL of 20% aqueous sodium thiosulfate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customto yield an oil
  6. filtrationThe oil was filtered through a plug of silica gel using 40% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-40f94f7d2fd243309b96b2bcfc7f32ac
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05434154

反応ノート

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