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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Potassium Carbonate → HCID 10430232、化合物

HRID 507822
ノート
印刷プレビュー

反応式

HRID 507822 の反応式
[CH2:1]([N:3]1[C:11](=[O:12])[C:10]2[N:9]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[CH:8]=[N:7][C:6]=2[NH:5][C:4]1=[O:22])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[C:29]([O:32][CH2:33][CH2:34]Br)(=[O:31])[CH3:30]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(#N)C>[C:29]([O:32][CH2:33][CH2:34][N:5]1[C:6]2[N:7]=[CH:8][N:9]([CH2:13][C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[C:10]=2[C:11](=[O:12])[N:3]([CH2:1][CH3:2])[C:4]1=[O:22])(=[O:31])[CH3:30]
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 11430Potassium CarbonateHCID 135641-Acetoxy-2-bromoethaneHCID 100657321-ethyl-3,7-dihydro-7-[(4-methoxyphenyl)methyl]-1H-Purine-2,6-dione

生成物 1

HCID 10430232HCID 10430232、化合物収率 75%

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒
HCID 6342
Acetonitrile
溶媒

実験手順

Acetonitrile was added to a mixture of Compound 5A (about 1.0 mole), anhydrous potassium carbonate (about 1.5 moles) and tetrabutylammonium hydrogen sulfate (about 0.05 mole). 2-bromoethyl acetate (about 1.5 moles) was added in three separate portions (0.72 mole in the beginning, another 0.45 mole after about 2 hours of reaction, and then the remaining 0.33 mole after about another 1 hour of reaction) during the course of the reaction at about 80-85° C. The total reaction time was about 7 hours. The reaction mixture was cooled to about room temperature and filtered. The filtrate was concentrated. Aqueous isopropanol was added to crystallize the product. The product was filtered, washed with aqueous isopropanol, and dried to provide Compound 6A in about a 75-80% yield.

後処理

  1. customseparate portions (0.72 mole in the beginning
  2. customanother 0.45 mole after about 2 hours of reaction
  3. customthe remaining 0.33 mole after about another 1 hour of reaction)
  4. customduring the course of the reaction at about 80-85° C
  5. temperatureThe reaction mixture was cooled to about room temperature
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. additionAqueous isopropanol was added
  9. customto crystallize the product
  10. filtrationThe product was filtered
  11. washwashed with aqueous isopropanol
  12. customdried

出典と根拠

ORDレコード
ord-e0a2568340c6469282b28d613c10dcef
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786301B2

反応ノート

読み込み中…

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