Sodium ethoxide → 2-ethoxy-4,6-bis[N-(2,2,6,6-tetramethyl-4-piperidinyl)butylamino]-1,3,5-triazine

HRID 1955966ノート

反応式

HRID 1955966 の反応式
[CH3:1][CH2:2][O-:3].[Na+].[CH3:5][C:6]1([CH3:41])[CH2:11][CH:10]([CH2:12][CH2:13][CH2:14][CH2:15][NH:16][C:17]2[N:22]=[C:21]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][CH:28]3[CH2:33][C:32]([CH3:35])([CH3:34])[NH:31][C:30]([CH3:37])([CH3:36])[CH2:29]3)[N:20]=[C:19](Cl)[N:18]=2)[CH2:9][C:8]([CH3:40])([CH3:39])[NH:7]1>C1(C)C=CC=CC=1>[CH2:2]([O:3][C:19]1[N:20]=[C:21]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][CH:28]2[CH2:33][C:32]([CH3:34])([CH3:35])[NH:31][C:30]([CH3:37])([CH3:36])[CH2:29]2)[N:22]=[C:17]([NH:16][CH2:15][CH2:14][CH2:13][CH2:12][CH:10]2[CH2:9][C:8]([CH3:40])([CH3:39])[NH:7][C:6]([CH3:41])([CH3:5])[CH2:11]2)[N:18]=1)[CH3:1]

参加物

4

反応物 2

HCID 2723922Sodium ethoxideHCID 190733162-chloro-4,6-bis[N-(2,2,6,6-tetramethylpiperidin-4-yl)butylamino]-s-triazine

生成物 1

HCID 675911962-ethoxy-4,6-bis[N-(2,2,6,6-tetramethyl-4-piperidinyl)butylamino]-1,3,5-triazine収率 74%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

g)1. 63.5 g (0. 195 mol) of a 21% solution of sodium ethylate in toluene are added dropwise at room temperature under nitrogen to a solution of 69.7 g (0.13 mol) of 2,4-bis[N-(2,2,6,6-tetramethyl-4-piperidinyl)butylamino]-6-chloro-1,3,5-triazine [EP-A-314 472, Sankyo] in 400 ml of toluene. The reaction mixture is then refluxed for 20 hours. After cooling to room temperature, the reaction mixture is washed successively with water, 1N sodium hydrogen carbonate solution and saturated sodium chloride solution. The organic phases are combined, dried over potassium carbonate and concentrated on a vacuum rotary evaporator. Crystallisation of the residue from acetonitrile gives 52.2 g (74%) of 2-ethoxy-4,6-bis[N-(2,2,6,6-tetramethyl-4-piperidinyl)butylamino]-1,3,5-triazine, m.p. 95°-104° C., in the form of a white powder. 1H-NMR (300 MHz, CDCl3): δ=4.345 ppm (q, J=7 Hz) --OCH2CH3.

後処理

  1. temperatureThe reaction mixture is then refluxed for 20 hours
  2. washthe reaction mixture is washed successively with water, 1N sodium hydrogen carbonate solution and saturated sodium chloride solution
  3. dry with materialdried over potassium carbonate
  4. concentrationconcentrated on a vacuum rotary evaporator
  5. customCrystallisation of the residue from acetonitrile

出典と根拠

ORDレコード
ord-1134b3e149cf4673bc049b240c0e17ac
出典データセット
uspto-grants-1998_07
特許番号
US05777113

反応ノート

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