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Lithium Hydroxide → HCID 18375083、化合物

HRID 2407697
ノート
印刷プレビュー

反応式

HRID 2407697 の反応式
[CH3:1][S:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:6]([C:16]([O:18]CC)=[O:17])=[CH:5][N:4]=1.[OH-].[Li+]>C(O)C>[NH:9]([C:7]1[C:6]([C:16]([OH:18])=[O:17])=[CH:5][N:4]=[C:3]([S:2][CH3:1])[N:8]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
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 2

HCID 3939Lithium HydroxideHCID 295672Ethyl 2-(methylthio)-4-(phenylamino)pyrimidine-5-carboxylate

生成物 1

HCID 18375083HCID 18375083、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl 2-(methylthio)-4-(phenylamino)pyrimidine-5-carboxylate (4.0 g, prepared according to the reported preparation in Barvian, M.; et al. J. Med. Chem. 2000, 43, 4606) in ethanol (50 mL) was treated with 2 N lithium hydroxide (50 mL) at room temperature for 16 hours. The reaction mixture was washed with ether and then brought to pH 6 via the addition of 1 N hydrochloric acid. The resulting precipitate was collected by filtration, azeotroped with toluene and dried under vacuum to obtain the title compound (2.2 g) having the following physical data.

後処理

  1. customaccording to the reported preparation in Barvian, M
  2. washThe reaction mixture was washed with ether
  3. additionbrought to pH 6 via the addition of 1 N hydrochloric acid
  4. filtrationThe resulting precipitate was collected by filtration
  5. customazeotroped with toluene
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-203e2b7f8663480e9c63d75165a276fa
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809538B2

反応ノート

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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