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

HRID 1463319
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HRID 1463319 반응식
[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]
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참가 물질

4

반응물 2

HCID 24640Iodine chlorideHCID 27781314-Amino-N-methylbenzenemethanesulfonamide

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-b5b224fbcd734a7b98c49a00b7d2c6b4
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05300506

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