ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

2-Bromoethyl methyl ether → 4-[4-(2-Methoxyethyl)piperazin-1-yl]-6-(3-trifluoromethylphenyl)-pyrimidine-2-carbonitrile trifluoroacetic acid salt

HRID 2053074
ノート
印刷プレビュー

反応式

HRID 2053074 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[N:8]1([C:14]2[CH:19]=[C:18]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=3)[N:17]=[C:16]([C:30]#[N:31])[N:15]=2)[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.C(N(C(C)C)CC)(C)C.Br[CH2:42][CH2:43][O:44][CH3:45].[N-]=C=O>C(#N)C>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[CH3:45][O:44][CH2:43][CH2:42][N:11]1[CH2:10][CH2:9][N:8]([C:14]2[CH:19]=[C:18]([C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:27])([F:28])[F:29])[CH:21]=3)[N:17]=[C:16]([C:30]#[N:31])[N:15]=2)[CH2:13][CH2:12]1
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 4

HCID 809722-Bromoethyl methyl etherHCID 81531DiisopropylethylamineHCID 105034IsocyanateHCID 866124954-(Piperazin-1-yl)-6-(3-trifluoromethylphenyl)-pyrimidine-2-carbonitrile trifluoroacetic acid salt

生成物 1

HCID 866124964-[4-(2-Methoxyethyl)piperazin-1-yl]-6-(3-trifluoromethylphenyl)-pyrimidine-2-carbonitrile trifluoroacetic acid salt

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirring solution of 4-(piperazin-1-yl)-6-(3-trifluoromethylphenyl)-pyrimidine-2-carbonitrile trifluoroacetic acid salt (Example 1; 100 mg) and diisopropylethylamine (78 μl) in acetonitrile (3 ml) was added 2-bromoethylmethylether (31 μl). The resulting solution was stirred at room temperature for 16 hrs, followed by heating at 45° C. for 24 hrs. Polymer bound isocyanate (1 mmol/g, 300 mg) was then added and the mixture was shaken at room temperature for 72 hrs before filtering and concentrating in vacuo. Residue was dissolved in dimethylsulphoxide and purified using the prep-HPLC to give 4-[4-(2-methoxyethyl)piperazin-1-yl]-6-(3-trifluoromethylphenyl)-pyrimidine-2-carbonitrile trifluoroacetic acid salt as a white solid (8 mg).

後処理

  1. temperatureby heating at 45° C. for 24 hrs
  2. additionwas then added
  3. stirringthe mixture was shaken at room temperature for 72 hrs
  4. filtrationbefore filtering
  5. concentrationconcentrating in vacuo
  6. dissolutionResidue was dissolved in dimethylsulphoxide
  7. custompurified

出典と根拠

ORDレコード
ord-d9e519ac139a4f30ace9fa9727986eeb
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07326715B2

反応ノート

読み込み中…

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