Cyanuric chloride → 2,4-Dichloro-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1yl)-1,3,5-triazine

HRID 345990ノート

反応式

HRID 345990 の反応式
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[CH2:10]1[CH2:23][O:22][C:12]2([CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14]([CH3:21])([CH3:20])[CH2:13]2)[O:11]1>C1(C)C(C)=CC=CC=1>[Cl:9][C:8]1[N:1]=[C:2]([Cl:3])[N:4]=[C:5]([N:15]2[C:16]([CH3:19])([CH3:18])[CH2:17][C:12]3([O:11][CH2:10][CH2:23][O:22]3)[CH2:13][C:14]2([CH3:21])[CH3:20])[N:7]=1

参加物

4

反応物 2

HCID 7954Cyanuric chlorideHCID 5670457,7,9,9-Tetramethyl-1,4-dioxa-8-azaspiro[4.5]decane

生成物 1

HCID 199917702,4-Dichloro-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1yl)-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒3 回

実験手順

A solution of 55.3 g (0.3 mol) of cyanuric chloride in 300 ml of xylene is added dropwise with stirring and cooling to 0°-5° to a solution of 119.6 g (0.6 mol) of 4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidine in 100 ml of xylene. The mixture is subsequently heated to reflux and kept at boiling point for 26 hours. After addition of 150 ml of xylene, the mixture is allowed to cool and the precipitate is filtered off. The filtrate is evaporated in vacuo. The residue is recrystallized from 300 ml of acetonitrile. The product obtained is a brownish powder which melts at 169°-172°.

後処理

  1. temperatureThe mixture is subsequently heated
  2. temperatureto reflux
  3. customfor 26 hours
  4. temperatureto cool
  5. filtrationthe precipitate is filtered off
  6. customThe filtrate is evaporated in vacuo
  7. customThe residue is recrystallized from 300 ml of acetonitrile
  8. customThe product obtained

出典と根拠

ORDレコード
ord-c7bb789d0b1d4f4bacfa19354d6ade46
出典データセット
uspto-grants-1991_10
特許番号
US05059689

反応ノート

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