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Benzaldehyde → HCID 67213120、化合物

HRID 2223827
ノート
印刷プレビュー

反応式

HRID 2223827 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH3:11])[CH3:10])[N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:3]=1.CN(C)C=O.[F:24][C:25]1[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=1[NH2:27].Cl.O1CCOCC1.C(O)C(N)(CO)CO.C(=O)C1C=CC=CC=1.C(=O)(O)[O-].[Na+]>CN1CCCC1=O.C(Cl)(Cl)Cl>[F:24][C:25]1[CH:31]=[CH:30][CH:29]=[CH:28][C:26]=1[NH:27][C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH3:11])[CH3:10])[N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:3]=1
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

9

反応物 6

HCID 240BenzaldehydeHCID 6503Tris(hydroxymethyl)aminomethaneHCID 516892Sodium BicarbonateHCID 7907666-Chloro-N2-isopropyl-N4-phenyl-1,3,5-triazine-2,4-diamineHCID 204431481,4-Dioxane hydrochlorideHCID 23033167HCID 23033167、化合物

生成物 1

HCID 67213120
HCID 67213120、化合物

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
80 °C

実験手順

A 14 mg portion of 6-chloro-N-isopropyl-N′-phenyl-1,3,5-triazine-2,4-diamine was dissolved in 800 μl of N-methyl-2-pyrrolidone, and 200 μl of 0.5 mM 2-fluoroaniline N,N-dimethylformamide solution and 50 μl of 4 M hydrochloric acid/dioxane were added thereto and stirred at 80° C. for 7 hours. After cooling down the reaction solution to 60° C., 50 mg (4.27 mmol/g) of PS-trisamine and 50 mg (1.53 mmol/g) of PS-benzaldehyde both manufactured by Algonote were added to the reaction solution and further stirred at 60° C. for 16 hours. The reaction solution was cooled down to room temperature and then mixed with saturated sodium bicarbonate aqueous solution and chloroform and stirred. After filtration of the solution, the organic layer was dried using anhydrous sodium sulfate, and then the solvent was evaporated under a reduced pressure to obtain 13 mg of N-(2-fluorophenyl)-N′-isopropyl-N″-phenyl-1,3,5-triazine-2,4,6-triamine as a brown resinous substance.

後処理

  1. temperatureAfter cooling down the reaction solution to 60° C.
  2. additionwere added to the reaction solution
  3. stirringfurther stirred at 60° C. for 16 hours
  4. temperatureThe reaction solution was cooled down to room temperature
  5. stirringstirred
  6. filtrationAfter filtration of the solution
  7. customthe organic layer was dried
  8. customthe solvent was evaporated under a reduced pressure

出典と根拠

ORDレコード
ord-adfed781310f452c884a0e15a1bcb7d7
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07375222B2

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