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Ammonium Chloride → 4-(2-Butynyloxy)-5-fluoro-6-(2,5-dimethyl-1-pyrrolidinyl)pyrimidine

HRID 2076843
ノート
印刷プレビュー

反応式

HRID 2076843 の反応式
[CH2:1]([O:5][C:6]1[C:11]([F:12])=[C:10](Cl)[N:9]=[CH:8][N:7]=1)[C:2]#[C:3][CH3:4].[CH3:14][CH:15]1[CH2:19][CH2:18][CH:17]([CH3:20])[NH:16]1.[Cl-].[NH4+]>>[CH2:1]([O:5][C:6]1[C:11]([F:12])=[C:10]([N:16]2[CH:17]([CH3:20])[CH2:18][CH2:19][CH:15]2[CH3:14])[N:9]=[CH:8][N:7]=1)[C:2]#[C:3][CH3:4]
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 25517Ammonium ChlorideHCID 960342,5-DimethylpyrrolidineHCID 225997174-(2-Butynyloxy)-5-fluoro-6-chloropyrimidine

生成物 1

HCID 593411414-(2-Butynyloxy)-5-fluoro-6-(2,5-dimethyl-1-pyrrolidinyl)pyrimidine収率 95.2%

実験手順

0.2 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine and 0.30 g of 2,5-dimethylpyrrolidine were mixed and left for 18 hours at room temperature. Into the reaction mixture was added a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.25 g of 4-(2-butynyloxy)-5-fluoro-6-(2,5-dimethyl-1-pyrrolidinyl)pyrimidine (hereinafter, referred to as Compound (6)).

後処理

  1. extractionthe mixture was extracted with tert-butyl methyl ether three times
  2. washThe organic layers were washed with a saturated sodium chloride aqueous solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-a5cee52dda254f0884fed738d2b53b17
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928110B2

反応ノート

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