Dimethyl Ether → HCID 178488689, 화합물

HRID 1296945노트

반응식

HRID 1296945 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:13]([CH3:14])=[N:12][N:11](COCC[Si](C)(C)C)[C:10]=2[C:23]2[CH:24]=[N:25][C:26]([NH2:29])=[N:27][CH:28]=2)=[CH:5][CH:4]=1.B(Cl)(Cl)Cl.COC.C([O-])(O)=O.[Na+]>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:13]([CH3:14])=[N:12][NH:11][C:10]=2[C:23]2[CH:28]=[N:27][C:26]([NH2:29])=[N:25][CH:24]=2)=[CH:5][CH:4]=1

참가 물질

6

반응물 4

HCID 8254Dimethyl EtherHCID 25135Boron TrichlorideHCID 516892Sodium BicarbonateHCID 58913495HCID 58913495, 화합물

생성물 1

HCID 178488689HCID 178488689, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

5-[4-(4-Methoxy-phenyl)-5-methyl-2-(2-trimethylsilanyl-ethoxymethyl)-2H-pyrazol-3-yl]-pyrimidin-2-ylamine was dissolved in anhydrous dichloromethane under nitrogen. 2M borontrichloride.dimethylether in dichloromethane (7 eq) was added dropwise, and all was stirred for 2 hours. The reaction mixture was added dropwise to sat. NaHCO3(aq) and extracted into dichloromethane. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. The residue was purified by preparative LC/MS to give 5-[4-(4-methoxy-phenyl)-5-methyl-2H-pyrazol-3-yl]-pyrimidin-2-ylamine as a solid.

후처리

  1. extractionextracted into dichloromethane
  2. dry with materialThe organic phase was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by preparative LC/MS

출처 및 근거

ORD 기록
ord-455d484964a3435bb8ae951d7731bec7
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07247734B2

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