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Cesium carbonate → 6-(4-(1H-1,2,4-triazol-1-yl)benzyl)-5-chloro-1-isobutyl-3-methyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione

HRID 2205657
ノート
印刷プレビュー

反応式

HRID 2205657 の反応式
[Cl:1][C:2]1[NH:3][CH:4]=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]([CH3:12])[C:7](=[O:13])[N:6]2[CH2:14][CH:15]([CH3:17])[CH3:16].Br[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([N:26]2[CH:30]=[N:29][CH:28]=[N:27]2)=[CH:22][CH:21]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.C(=O)(O)[O-].[Na+]>[N:26]1([C:23]2[CH:24]=[CH:25][C:20]([CH2:19][N:3]3[C:2]([Cl:1])=[C:10]4[C:5]([N:6]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:7](=[O:13])[N:8]([CH3:12])[C:9]4=[O:11])=[CH:4]3)=[CH:21][CH:22]=2)[CH:30]=[N:29][CH:28]=[N:27]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 27764891-(4-(bromomethyl)phenyl)-1H-1,2,4-triazoleHCID 67415912HCID 67415912、化合物

生成物 1

HCID 701128166-(4-(1H-1,2,4-triazol-1-yl)benzyl)-5-chloro-1-isobutyl-3-methyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione収率 96.9%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 516892
Sodium Bicarbonate
溶媒

実験手順

A suspension of 5-chloro-1-isobutyl-3-methyl-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (103 mg, 0.4 mmol), 1-(4-(bromomethyl)phenyl)-1H-1,2,4-triazole (93 mg, 0.48 mmol) and cesium carbonate (195 mg, 0.6 mmol) in anhydrous DMF (3 mL) is stirred at room temperature for 3 hours. The mixture is diluted with 20 mL of saturated sodium bicarbonate, and then extracted with CH2Cl2 three times. The combined organic phase is washed with brine, and then dried with anhydrous Na2SO4. After filtration through celite, the filtrate is concentrated to dryness under vacuum to give 160 mg of crude product as light brown solids, which is used in the next step without further purification. MS (ESI) m/z 413.2 [M+H]+.

後処理

  1. extractionextracted with CH2Cl2 three times
  2. washThe combined organic phase is washed with brine
  3. dry with materialdried with anhydrous Na2SO4
  4. filtrationAfter filtration through celite
  5. concentrationthe filtrate is concentrated to dryness under vacuum

出典と根拠

ORDレコード
ord-562e790218754594af60508044b0b106
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09371327B2

反応ノート

読み込み中…

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