Dimethylformamide → HCID 10204670、化合物

HRID 1591698ノート

反応式

HRID 1591698 の反応式
COC(=O)[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:35].[K+].[K+].C[N:41]([CH:43]=[O:44])C>>[CH:17]1([CH2:16][O:15][C:12]2[CH:11]=[CH:10][C:9]([S:6]([N:5]([CH2:4][C:43]([NH:41][OH:35])=[O:44])[CH2:22][C:23]3[CH:28]=[CH:27][C:26]([N:29]4[N:33]=[CH:32][CH:31]=[N:30]4)=[CH:25][CH:24]=3)(=[O:7])=[O:8])=[CH:14][CH:13]=2)[CH2:18][CH2:19]1

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 219436922-(4-Chloromethyl-phenyl)-2h-[1,2,3]triazoleHCID 68686408HCID 68686408、化合物

生成物 1

HCID 10204670HCID 10204670、化合物

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-fe32f782ce0f47c19999370b0084503f
出典データセット
uspto-grants-2007_11
特許番号
US07291634B2

反応ノート

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