4-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile monohydrochloride monohydrate → 4-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile

HRID 1062551ノート

反応式

HRID 1062551 の反応式
O.Cl.[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:5]=1[CH2:11][C:12]1[N:17]=[C:16]([NH:18][OH:19])[N:15]=[C:14]([NH:20][C:21]2[CH:28]=[CH:27][C:24]([C:25]#[N:26])=[CH:23][CH:22]=2)[N:13]=1>C(OC(=O)C)C>[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:5]=1[CH2:11][C:12]1[N:17]=[C:16]([NH:18][OH:19])[N:15]=[C:14]([NH:20][C:21]2[CH:22]=[CH:23][C:24]([C:25]#[N:26])=[CH:27][CH:28]=2)[N:13]=1

参加物

3

反応物 1

HCID 222816854-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile monohydrochloride monohydrate

生成物 1

HCID 4864294-[[4-[(2,6-Dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile収率 70.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

Compound (21) (0.00227 mol) was stirred in ethylacetate (50 ml). The mixture was washed with NaHCO3 (50 ml saturated solution), then washed with brine, dried, filtered and the solvent was evaporated. The residue was crystallized from methanol, filtered off and dried, yielding 0.60 g (70.6%) of 4-[[4-[(2,6-dichlorophenyl)methyl]-6-(hydroxyamino)-1,3,5-triazin-2-yl]amino]benzonitrile (compound 33).

後処理

  1. washThe mixture was washed with NaHCO3 (50 ml saturated solution)
  2. washwashed with brine
  3. customdried
  4. filtrationfiltered
  5. customthe solvent was evaporated
  6. customThe residue was crystallized from methanol
  7. filtrationfiltered off
  8. customdried

出典と根拠

ORDレコード
ord-97a7978ffcc141c78bf0e126a2ff33c6
出典データセット
uspto-grants-2005_11
特許番号
US06962916B2

反応ノート

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