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

HRID 527377노트

반응식

HRID 527377 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 867116434-(N,S-Dimethylsulfonimidoyl)benzylamine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-e79c3980c4ee481c8d121f645d85ca49
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346794B1

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