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Ethyl Acetate → 2-Chloro-4-[4-methoxymethyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-benzonitrile

HRID 2233593
ノート
印刷プレビュー

反応式

HRID 2233593 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:28]=[CH:29][C:30]=1[C:31]#[N:32])[O:5][CH2:6][C:7]1[S:11][C:10]([C:12]2[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:20])[F:19])=[CH:14][CH:13]=2)=[N:9][C:8]=1[CH2:22][O:23]S(C)(=O)=O.C[O-].[Na+].[C:36](OCC)(=O)C>CO>[Cl:1][C:2]1[CH:3]=[C:4]([O:5][CH2:6][C:7]2[S:11][C:10]([C:12]3[CH:17]=[CH:16][C:15]([C:18]([F:21])([F:19])[F:20])=[CH:14][CH:13]=3)=[N:9][C:8]=2[CH2:22][O:23][CH3:36])[CH:28]=[CH:29][C:30]=1[C:31]#[N:32]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 10942334Sodium MethoxideHCID 59296164Methanesulfonic acid 5-(3-chloro-4-cyano-phenoxymethyl)-2-(4-trifluoromethyl-phenyl)-thiazol-4-ylmethyl ester

生成物 1

HCID 592961972-Chloro-4-[4-methoxymethyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-benzonitrile

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

120 mg Methanesulfonic acid 5-(3-chloro-4-cyano-phenoxymethyl)-2-(4-trifluoromethyl-phenyl)-thiazol-4-ylmethyl ester were dissolved in 5 ml methanol. 12.9 mg sodium methoxide were added and the mixture stirred at 50° C. for one hour. The reaction mixture was diluted by addition of 50 ml ethyl acetate, washed with one molar hydrochloric acid then dried over MgSO4. The solvent was removed in vacuo and the residue purified by RP-HPLC to provide 30 mg of 2-chloro-4-[4-methoxymethyl-2-(4-trifluoromethyl-phenyl)-thiazol-5-ylmethoxy]-benzonitrile as lyophilisate.

後処理

  1. washwashed with one molar hydrochloric acid
  2. dry with materialthen dried over MgSO4
  3. customThe solvent was removed in vacuo
  4. customthe residue purified by RP-HPLC

出典と根拠

ORDレコード
ord-91b4b21b6ceb455192e48ceac4f635e5
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709509B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート