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Hydrochloric Acid → 5-(4-Iodo-phenyl)-7-methylsulfanyl-pyrazolo[1,5-c]pyrimidine

HRID 19610
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HRID 19610 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:13][C:12](=[S:14])[N:11]3[N:15]=[CH:16][CH:17]=[C:10]3[CH:9]=2)=[CH:4][CH:3]=1.Cl.[CH3:19]O>[OH-].[Na+].CI>[I:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:13]=[C:12]([S:14][CH3:19])[N:11]3[N:15]=[CH:16][CH:17]=[C:10]3[CH:9]=2)=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 178527901HCID 178527901, 화합물2회

생성물 1

HCID 673194195-(4-Iodo-phenyl)-7-methylsulfanyl-pyrazolo[1,5-c]pyrimidine수율 62%

시약·촉매·용매 2

HCID 6328Methyl iodide용매2회HCID 14798
Sodium Hydroxide
용매

실험 절차

To a solution of 5-(4-iodo-phenyl)-6H-pyrazolo[1,5-c]pyrimidine-7-thione (compound E1)(2.09 g) in 2M aqueous NaOH (3 ml) and methanol (40 ml), methyl iodide (0.376 ml) is added at ambient temperature. After 30 min at this temperature further methyl iodide (0.376 ml) is added. After 60 min the mixture is neutralized with 2M hydrochloric acid and evaporated. The residue is partitioned between dichloromethane and water and the organic phase is washed twice with water. The organic phase is dried over sodium sulfate and the crude product is purified by silica gel flash chromatography. A nearly colorless solid (1.35 g, 62%) is obtained.

후처리

  1. customevaporated
  2. customThe residue is partitioned between dichloromethane and water
  3. washthe organic phase is washed twice with water
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customthe crude product is purified by silica gel flash chromatography

출처 및 근거

ORD 기록
ord-b247128ee3224d0c91cfed75187bcfd9
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07745446B2

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