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

HRID 1694850
ノート
印刷プレビュー

反応式

HRID 1694850 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-75b327c996ab4bf1b52953676a138120
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158825B2

反応ノート

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