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Sodium Hydroxide → N'-[6-(4-chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-yl]-N-ethyl-N-methyl-formamidine

HRID 1894640
ノート
印刷プレビュー

反応式

HRID 1894640 の反応式
[CH2:1]([N:3]([CH3:6])[CH:4]=O)[CH3:2].[Cl-].[P+]=O.[Cl:10][C:11]1[CH:31]=[CH:30][C:14]([O:15][C:16]2[N:21]=[C:20]([CH3:22])[C:19]([NH2:23])=[CH:18][C:17]=2[C:24]#[C:25][Si:26]([CH3:29])([CH3:28])[CH3:27])=[CH:13][C:12]=1[C:32]([F:35])([F:34])[F:33].[OH-].[Na+]>ClCCl>[Cl:10][C:11]1[CH:31]=[CH:30][C:14]([O:15][C:16]2[N:21]=[C:20]([CH3:22])[C:19]([N:23]=[CH:4][N:3]([CH2:1][CH3:2])[CH3:6])=[CH:18][C:17]=2[C:24]#[C:25][Si:26]([CH3:29])([CH3:27])[CH3:28])=[CH:13][C:12]=1[C:32]([F:34])([F:33])[F:35]
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 14798Sodium HydroxideHCID 350667N-ethyl-N-methylformamideHCID 581534926-(4-Chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-ylamineHCID 178527006HCID 178527006、化合物

生成物 1

HCID 25159299N'-[6-(4-chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-yl]-N-ethyl-N-methyl-formamidine

試薬・触媒・溶媒

1
HCID 6344Dichloromethane溶媒2 回

実験手順

In a 10 ml single-necked round-bottomed flask, 3.1 mg. of ethylmethylformamide is solubilized in 0.25 ml of dry dichloromethane at ambient temperature (colourless solution). Under stirring, 0.0032 ml of phosphorous oxide chloride is added dropwise by syringe. Stirring at ambient temperature is continued for 1.0 hour, whereupon a pink-orange solution is obtained. To this solution, 7.0 mg of 6-(4-chloro-3-trifluoromethyl-phenoxy)-2-methyl-5-trimethylsilanylethynyl-pyridin-3-ylamine dissolved in 0.75 ml of dry dichloromethane is added dropwise by syringe, giving a yellow solution. Stirring is continued at room temperature for 2.5 hours. The mixture is then poured into ice/water (pH=2, water phase). 2 M aqueous NaOH is then added to get a pH of about 11 and stirring is continued for 15 minutes. The mixture is then extracted with two 10 ml portions of diethyl ether. The combined organic phases are then dried over sodium sulfate, filtered and the solvent is removed in vacuo to obtain 6.0 mg of the compound as a yellow oil. RP HPLC: retention time of compound: 1.61 minutes.

後処理

  1. stirringStirring at ambient temperature
  2. customis obtained
  3. additionis added dropwise by syringe
  4. customgiving a yellow solution
  5. stirringStirring
  6. waitis continued at room temperature for 2.5 hours
  7. customto get a pH of about 11
  8. stirringstirring
  9. waitis continued for 15 minutes
  10. extractionThe mixture is then extracted with two 10 ml portions of diethyl ether
  11. dry with materialThe combined organic phases are then dried over sodium sulfate
  12. filtrationfiltered
  13. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-9f264b347a48407fba57eed7b65c35a0
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08513286B2

反応ノート

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