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Nitrogen → 2-Methanesulfonyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

HRID 1694850
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반응식

HRID 1694850 반응식
[CH3:1][O:2][C:3]([C:5]1[S:18][C:8]2[N:9]=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[N:11]=[C:12](Cl)[C:7]=2[CH:6]=1)=[O:4].N#N>C1COCC1.CO.[Pd]>[CH3:1][O:2][C:3]([C:5]1[S:18][C:8]2[N:9]=[C:10]([S:14]([CH3:17])(=[O:16])=[O:15])[N:11]=[CH:12][C:7]=2[CH:6]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 947NitrogenHCID 593764254-Chloro-2-methanesulfonyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

생성물 1

HCID 593764492-Methanesulfonyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a solution of 4-chloro-2-methanesulfonyl-thieno[2,3-d]pyrimidine-6-carboxylic acid methyl ester (700 mg, 2.2 mmol) in THF/MeOH (10/10 mL) purged with N2 was added Pd/C (700 mg). The reaction mixture was purged with N2, evacuated and purged with H2 three times. After 6 h, the mixture was filtered via Celite and concentrated. The residue dissolved in MeOH/CH2Cl2 and the solid was filtered. The filtrate containing the product was concentrated and used without further purification. ESIMS calcd 273 (M++H), found 273 (M++H).

후처리

  1. customThe reaction mixture was purged with N2
  2. customevacuated
  3. custompurged with H2 three times
  4. filtrationthe mixture was filtered via Celite
  5. concentrationconcentrated
  6. dissolutionThe residue dissolved in MeOH/CH2Cl2
  7. filtrationthe solid was filtered
  8. additionThe filtrate containing the product
  9. concentrationwas concentrated
  10. customused without further purification

출처 및 근거

ORD 기록
ord-75b327c996ab4bf1b52953676a138120
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08158825B2

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