Ethylenediamine → 4-(N,S-Dimethylsulfonimidoyl)benzylamine

HRID 527377ノート

反応式

HRID 527377 の反応式
[CH3:1][N:2]=[S:3]([C:6]1[CH:23]=[CH:22][C:9]([CH2:10][N:11]2C(=O)C3C(=CC=CC=3)C2=O)=[CH:8][CH:7]=1)([CH3:5])=[O:4].NCCN.C(#N)C.O1CCCC1>C(O)C>[CH3:1][N:2]=[S:3]([C:6]1[CH:23]=[CH:22][C:9]([CH2:10][NH2:11])=[CH:8][CH:7]=1)([CH3:5])=[O:4]

参加物

6

反応物 4

HCID 3301EthylenediamineHCID 6342AcetonitrileHCID 8028TetrahydrofuranHCID 867116422-(4-(N,S-Dimethylsulfonimidoyl)benzyl)isoindoline-1,3-dione

生成物 1

HCID 867116434-(N,S-Dimethylsulfonimidoyl)benzylamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-(4-(N,S-dimethylsulfonimidoyl)benzyl)isoindoline-1,3-dione (189 mg, 0.58 mmol) and 1,2-diaminoethane (132 μL, 3.44 mmol) in a 2:1:1 mixture of acetonitrile, tetrahydrofuran and ethanol (2 mL) is heated at reflux for 1 h. All volatiles are removed under reduced pressure, and the residue is treated with dichloromethane. The mixture is filtered, and the filtrate is concentrated under reduced pressure. Yield: 114 mg (85% of theory); ESI mass spectrum: [M+H]+=199; r.t. HPLC: 0.22 min (X011_S03).

後処理

  1. temperatureis heated
  2. temperatureat reflux for 1 h
  3. customAll volatiles are removed under reduced pressure
  4. additionthe residue is treated with dichloromethane
  5. filtrationThe mixture is filtered
  6. concentrationthe filtrate is concentrated under reduced pressure
  7. customr.t
  8. custom0.22 min (X011_S03)

出典と根拠

ORDレコード
ord-e79c3980c4ee481c8d121f645d85ca49
出典データセット
uspto-grants-2016_05
特許番号
US09346794B1

反応ノート

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