Potassium Carbonate → HCID 68683130、化合物

HRID 2216661ノート

反応式

HRID 2216661 の反応式
[CH3:1][O:2][C:3](=[O:20])[CH2:4][NH:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH:17]2[CH2:19][CH2:18]2)=[CH:11][CH:10]=1)(=[O:8])=[O:7].Cl[CH2:22][C:23]1[CH:28]=[CH:27][C:26]([N:29]2[N:33]=[CH:32][CH:31]=[N:30]2)=[CH:25][CH:24]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:1][O:2][C:3](=[O:20])[CH2:4][N:5]([S:6]([C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH:17]2[CH2:18][CH2:19]2)=[CH:11][CH:10]=1)(=[O:7])=[O:8])[CH2:22][C:23]1[CH:24]=[CH:25][C:26]([N:29]2[N:30]=[CH:31][CH:32]=[N:33]2)=[CH:27][CH:28]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 219436922-(4-Chloromethyl-phenyl)-2h-[1,2,3]triazoleHCID 68686408HCID 68686408、化合物

生成物 1

HCID 68683130HCID 68683130、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1 g (3.3 mmol) of the compound of Stage 3.7 in 10 ml of DMF, 0.8086 g (4.175 mmol) of 2-(4-chloromethyl-phenyl)-2H-[1,2,3]triazole, 0.0555 g (0.33 mmol) of KI and 0.646 g (4.68 mmol) of K2CO3 are added successively at r.t. After stirring for 18 h, the reaction is quenched with ice water and the mixture is extracted with AcOEt. The combined extracts are washed with H2O, brine, dried over MgSO4 and concentrated under reduced pressure to give a solid which is washed with diethylether and MeOH to give the title compound.

後処理

  1. customthe reaction is quenched with ice water
  2. extractionthe mixture is extracted with AcOEt
  3. washThe combined extracts are washed with H2O, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customto give a solid which
  7. washis washed with diethylether and MeOH

出典と根拠

ORDレコード
ord-34197964acb94e889b7db05ac7affbae
出典データセット
uspto-grants-2006_09
特許番号
US07112611B2

反応ノート

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