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Cesium carbonate → 1-(2-Fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-d]pyrimidine

HRID 570538
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HRID 570538 반응식
[I:1][C:2]1[C:10]2[C:5](=[N:6][CH:7]=[N:8][CH:9]=2)[NH:4][N:3]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[F:17][C:18]1[CH:25]=[CH:24][CH:23]=[CH:22][C:19]=1[CH2:20]Br>CN(C=O)C.O>[F:17][C:18]1[CH:25]=[CH:24][CH:23]=[CH:22][C:19]=1[CH2:20][N:4]1[C:5]2=[N:6][CH:7]=[N:8][CH:9]=[C:10]2[C:2]([I:1])=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 67968alpha-Bromo-o-fluorotolueneHCID 178506576HCID 178506576, 화합물

생성물 1

HCID 866921041-(2-Fluorobenzyl)-3-iodo-1H-pyrazolo[3,4-d]pyrimidine수율 89.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매2회
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실험 절차

569 mg (2.313 mmol) of 3-iodo-1H-pyrazolo[3,4-d]pyrimidine and 828 mg (2.544 mmol) of caesium carbonate were initially charged in 10 ml of DMF, and 481 mg (2.544 mmol) of 2-fluorobenzyl bromide dissolved in 2 ml of DMF were added. The reaction mixture was stirred at RT overnight, diluted with 50 ml of water and filtered with suction, and the residue was dried under high vacuum. 733 mg of the target compound were obtained (purity 83%; 74% of theory).

후처리

  1. additionwere added
  2. filtrationfiltered with suction
  3. customthe residue was dried under high vacuum

출처 및 근거

ORD 기록
ord-64df922a521f4246bdf9bcf7c4a82a29
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09023849B2

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