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Acetic Acid → 1-methyl-3-pentyl-3,7-dihydro-1H-purine-2,6-dione

HRID 2386641
ノート
印刷プレビュー

反応式

HRID 2386641 の反応式
[CH3:1][N:2]1[C:10](=[O:11])[C:9]2[N:8](CC=C)[CH:7]=[N:6][C:5]=2[N:4]([CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[C:3]1=[O:20].C1([SiH3])C=CC=CC=1.C(O)(=O)C>C(Cl)Cl.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:1][N:2]1[C:10](=[O:11])[C:9]2[NH:8][CH:7]=[N:6][C:5]=2[N:4]([CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[C:3]1=[O:20]
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 176Acetic AcidHCID 12752PhenylsilaneHCID 592995971-methyl-3-pentyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione

生成物 1

HCID 248477161-methyl-3-pentyl-3,7-dihydro-1H-purine-2,6-dione

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 6344
Dichloromethane
溶媒

実験手順

1-methyl-3-pentyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (0.45 g, 1.63 mmol), phenylsilane (0.25 ml, 2.03 mmol) and tetrakis(triphenylphosphine)palladium(0) (0.35 g, 0.3 mmol) was dissolved in DCM (10 ml) containing acetic acid (6 ml). The air in the flask was replaced by nitrogen by evacuating the flask then filling with nitrogen (×3) and the reaction mixture heated to 45 C for 4 h. The solution was allowed to cool diluted with DCM then washed with water then saturated sodium bicarbonate solution. The organics were isolated, dried and concentrated to yield crude product. Purification by SPE (silica) eluting with ether provided the product, 0.06 g, 16%. m/z 237 [MH+].

後処理

  1. customby evacuating the flask
  2. temperaturethe reaction mixture heated to 45 C for 4 h
  3. temperatureto cool
  4. additiondiluted with DCM
  5. washthen washed with water
  6. customThe organics were isolated
  7. customdried
  8. concentrationconcentrated
  9. customto yield crude product
  10. customPurification by SPE (silica)
  11. washeluting with ether
  12. customprovided the product, 0.06 g, 16%

出典と根拠

ORDレコード
ord-2d6d7a3bc4484ed1a3698d70d5153fb2
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268839B2

反応ノート

読み込み中…

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