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Tetrafluoro-m-phenylenediamine dihydrochloride → 2-[4-(p-Methoxyphenyl)-1-piperazinyl]-4,6-bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazine

HRID 2287156
ノート
印刷プレビュー

反応式

HRID 2287156 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]([CH3:15])([CH3:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[N:5]=[C:4]([NH:16][C:17]([CH3:23])([CH3:22])[C:18]([CH3:21])([CH3:20])[CH3:19])[N:3]=1.[CH3:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([N:32]2[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]2)=[CH:28][CH:27]=1.C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl>ClC1C=CC=CC=1>[CH3:24][O:25][C:26]1[CH:27]=[CH:28][C:29]([N:32]2[CH2:37][CH2:36][N:35]([C:2]3[N:7]=[C:6]([NH:8][C:9]([CH3:15])([CH3:14])[C:10]([CH3:13])([CH3:11])[CH3:12])[N:5]=[C:4]([NH:16][C:17]([CH3:22])([CH3:23])[C:18]([CH3:19])([CH3:21])[CH3:20])[N:3]=3)[CH2:34][CH2:33]2)=[CH:30][CH:31]=1
参加物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 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 2697221-(4-Methoxyphenyl)piperazineHCID 155725772-Chloro-4,6-di(2,3,3-trimethyl-2-butyl)amino-s-triazine

生成物 1

HCID 234594992-[4-(p-Methoxyphenyl)-1-piperazinyl]-4,6-bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazine

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

A mixture of 6.84 g. of 2-chloro-4,6-bis[(1,1,2,2-tetramethylpropyl)amino]-s-triazine and 7.69 g. of N-(p-methoxyphenyl)piperazine (prepared from the commercially available dihydrochloride salt) in 150 ml. of chlorobenzene is refluxed for 5 hours and then cooled. The reaction mixture is washed with two 25 ml. portions of water. The organic layer is dried over anhydrous potassium carbonate and magnesium sulfate and the solvent is stripped with a water pump. The residual amber oil is crystallized by slurrying in isopropanol. Recrystallization from 150 ml. of propanol (using charcoal for decolorization) gives the desired product as a white solid, m.p. 155°-157° C.

後処理

  1. additionA mixture of 6.84 g
  2. temperaturecooled
  3. washThe reaction mixture is washed with two 25 ml
  4. dry with materialThe organic layer is dried over anhydrous potassium carbonate and magnesium sulfate
  5. customThe residual amber oil is crystallized
  6. customRecrystallization from 150 ml

出典と根拠

ORDレコード
ord-11fdc509d712497a98bb0c44693b631a
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04269832

反応ノート

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