Hydrochloric Acid → HCID 21867183、化合物

HRID 857126ノート

反応式

HRID 857126 の反応式
[I:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:12][C:11](=[O:13])[NH:10][C:9]2=[O:14])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].[CH2:17](Br)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.Cl>CN(C=O)C>[CH2:17]([N:10]1[C:11](=[O:13])[CH2:12][N:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([I:1])[CH:3]=2)[C:9]1=[O:14])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 218671771-(3-Iodophenyl)-2,4-imidazolidinedione

生成物 1

HCID 21867183HCID 21867183、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-(3-Iodophenyl)imidazolidine-2,4-dione (0.5 g) was taken up in dry DMF (10 ml) and treated with sodium hydride (60% oil dispersion, 73 mg) and stirred for 20 min under nitrogen. Benzyl bromide (0.295 ml) was added and stirring continued for 3 h. 2M HCl (100 ml) was added and the mixture extracted with EtOAc. The combined extracts were washed with saturated aqueous sodium hydrogen carbonate (50 ml), brine (50 ml) and dried (MgSO4). This was recrystallised from MeOH to give the title compound (0.255 g). LCMS RT 3.53 min.

後処理

  1. stirringstirring
  2. waitcontinued for 3 h
  3. extractionthe mixture extracted with EtOAc
  4. washThe combined extracts were washed with saturated aqueous sodium hydrogen carbonate (50 ml), brine (50 ml)
  5. dry with materialdried (MgSO4)
  6. customThis was recrystallised from MeOH

出典と根拠

ORDレコード
ord-dcd6f19d0f474d478dc5b878332a5e60
出典データセット
uspto-grants-2006_12
特許番号
US07144908B2

反応ノート

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