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Sodium Hydroxide → 2-Butyl-4-chloro-5H-pyrrolo[3,2-d]pyrimidine

HRID 1487242
ノート
印刷プレビュー

反応式

HRID 1487242 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([C:10]1[NH:11][C:12](=O)[C:13]2[NH:18][CH:17]=[CH:16][C:14]=2[N:15]=1)[CH2:7][CH2:8][CH3:9].[OH-].[Na+]>>[CH2:6]([C:10]1[N:11]=[C:12]([Cl:3])[C:13]2[NH:18][CH:17]=[CH:16][C:14]=2[N:15]=1)[CH2:7][CH2:8][CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 1370052332-Butyl-3H-pyrrolo[3,2-d]pyrimidin-4(5H)-one

生成物 1

HCID 1183828482-Butyl-4-chloro-5H-pyrrolo[3,2-d]pyrimidine収率 91.2%

実験手順

Phosphorus oxychloride (20 mL, 21.46 mmol) was added to 2-butyl-3H-pyrrolo[3,2-d]pyrimidin-4(5H)-one (1.69 g). The resultant mixture was heated at 100° C. After 4 hours the reaction mixture was cooled to room temperature then poured onto ice. The aqueous phase was treated with aqueous sodium hydroxide solution (5M) until the pH was 7. The resultant mixture was extracted with ethyl acetate (2×150 mL). The combined organic phase were washed with brine, dried (Na2SO4), filtered and evaporated to give the title compound (1.69 g)

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  1. additionthen poured onto ice
  2. extractionThe resultant mixture was extracted with ethyl acetate (2×150 mL)
  3. washThe combined organic phase were washed with brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-ae5c141428364f578ce378acafbd3d39
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428512B2

反応ノート

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