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 270631

反応式

HRID 270631 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-f688cf125a5448d287e4e8b0016167c6
出典データセット
uspto-grants-2008_11
特許番号
US07449575B2

関連ノート

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