Dimethylformamide → HCID 10204670, 화합물

HRID 1591698노트

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HRID 1591698 반응식
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

참가 물질

5

반응물 4

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

생성물 1

HCID 10204670HCID 10204670, 화합물

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fe32f782ce0f47c19999370b0084503f
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07291634B2

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