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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
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HRID 2287156 반응식
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
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참가 물질

5

반응물 3

HCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 2697221-(4-Methoxyphenyl)piperazineHCID 155725772-Chloro-4,6-di(2,3,3-trimethyl-2-butyl)amino-s-triazine

생성물 1

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

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-11fdc509d712497a98bb0c44693b631a
출처 데이터셋
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04269832

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