Sodium Sulfite → Tert-butyl 2-(methylsulfonyl)-5H-pyrrolo[3,4-D]pyrimidine-6(7H)-carboxylate

HRID 546439ノート

反応式

HRID 546439 の反応式
Cl[C:2]1C=CC=C(C(OO)=O)C=1.[C:12]([O:16][C:17]([N:19]1[CH2:27][C:26]2[CH:25]=[N:24][C:23](SC)=[N:22][C:21]=2[CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].[S:30]([O-:33])([O-])=[O:31].[Na+].[Na+].C(=O)([O-])O.[Na+]>ClCCl>[C:12]([O:16][C:17]([N:19]1[CH2:27][C:26]2[CH:25]=[N:24][C:23]([S:30]([CH3:2])(=[O:33])=[O:31])=[N:22][C:21]=2[CH2:20]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

参加物

6

反応物 4

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 18442822Tert-butyl 2-(methylthio)-5H-pyrrolo[3,4-D]pyrimidine-6(7H)-carboxylate

生成物 1

HCID 18442821Tert-butyl 2-(methylsulfonyl)-5H-pyrrolo[3,4-D]pyrimidine-6(7H)-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

m-Chloroperbenzoic acid (1.99 g) was added to a dichloromethane solution (20 ml) of 6-(tert-butoxy-carbonyl)-5,7-dihydro-2-methylthiopyrrolo[3,4-d]-pyrimidine (1.08 g) under ice cooling, and the mixture was stirred for 5 hours. A saturated aqueous solution of sodium sulfite, a saturated aqueous solution of sodium hydrogen carbonate and dichloromethane were added to separate an organic layer. The organic layer was then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, hexane was added to the residue, and powder deposited was collected by filtration to obtain the title compound (1.09 g) as colorless powder.

後処理

  1. customto separate an organic layer
  2. dry with materialThe organic layer was then dried over anhydrous sodium sulfate
  3. distillationThe solvent was distilled off under reduced pressure, hexane
  4. additionwas added to the residue, and powder
  5. filtrationdeposited was collected by filtration

出典と根拠

ORDレコード
ord-28ee22c8276b41038e9c2c083a1e5682
出典データセット
uspto-grants-2011_05
特許番号
US07935824B2

反応ノート

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