Dimethylformamide dimethyl acetal → 4-[[4-[(2,6-Dichlorophenyl)methyl]-6-[[(dimethylamino)methylene]amino]-1,3,5-triazin-2-yl]amino]benzonitrile

HRID 25055

反応式

HRID 25055 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([CH2:8][C:9]2[C:14]([Cl:15])=[CH:13][CH:12]=[CH:11][C:10]=2[Cl:16])[N:5]=[C:4]([NH:17][C:18]2[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[CH:20][CH:19]=2)[N:3]=1.CO[CH:28](OC)[N:29]([CH3:31])[CH3:30]>>[Cl:16][C:10]1[CH:11]=[CH:12][CH:13]=[C:14]([Cl:15])[C:9]=1[CH2:8][C:6]1[N:7]=[C:2]([N:1]=[CH:28][N:29]([CH3:31])[CH3:30])[N:3]=[C:4]([NH:17][C:18]2[CH:19]=[CH:20][C:21]([C:22]#[N:23])=[CH:24][CH:25]=2)[N:5]=1

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 4863624-[[4-Amino-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]amino]benzonitrile

生成物 1

HCID 4864454-[[4-[(2,6-Dichlorophenyl)methyl]-6-[[(dimethylamino)methylene]amino]-1,3,5-triazin-2-yl]amino]benzonitrile

実験手順

Compound (1) (0.0016 mol) and 1,1-dimethoxy-N,N-dimethylmethanamine (21 ml) were combined and stirred vigorously at ambient temperature for 8 hours. The reaction mixture was filtered and the collected solid was washed with ether (Fraction A). Additional compound was obtained by concentration of the filtrate (Fraction B). Fractions A and B were combined and recrystallized from ethanol, yielding 0.15 g of 4-[[4-[(2,6-dichlorophenyl)methyl]-6-[[(dimethylamino)methylene]amino]-1,3,5-triazin-2-yl]amino]benzonitrile (compound 62).

後処理

  1. filtrationThe reaction mixture was filtered
  2. washthe collected solid was washed with ether (Fraction A)
  3. customAdditional compound was obtained by concentration of the filtrate (Fraction B)
  4. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-039fc777b0a64bfcba2822c0ace28a59
出典データセット
uspto-grants-2005_02
特許番号
US06858609B2

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