Glycinamide → 2-[[4-(4-Cyanoanilino)-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]amino]acetamide

HRID 270629

反応式

HRID 270629 の反応式
Cl[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.[NH2:26][CH2:27][C:28]([NH2:30])=[O:29].C(N(CC)C(C)C)(C)C>O1CCOCC1>[C:22]([C:21]1[CH:20]=[CH:19][C:18]([NH:17][C:4]2[N:5]=[C:6]([CH2:8][C:9]3[C:14]([Cl:15])=[CH:13][CH:12]=[CH:11][C:10]=3[Cl:16])[N:7]=[C:2]([NH:26][CH2:27][C:28]([NH2:30])=[O:29])[N:3]=2)=[CH:25][CH:24]=1)#[N:23]

参加物

5

反応物 3

HCID 69020GlycinamideHCID 81531DiisopropylethylamineHCID 4864234-[[4-Chloro-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]amino]benzonitrile

生成物 1

HCID 5054092-[[4-(4-Cyanoanilino)-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]amino]acetamide収率 41.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Intermediate (27) (0.00423 mol), 2-amino-acetamide (0.00431 mol), 1,4-dioxane (20 ml) and N,N-diisopropylethylamine (0.00862 mol) were combined and stirred at RT for 16 hours under argon. The reaction mixture was quenched with H2O and filtered. The residue was washed with H2O, filtered and recrystallized from ACN (200 ml). The precipitate was filtered off and dried, yielding 0.75 g (41.4%) of [N-[4-[(4-cyano-phenyl)amino]-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]]aminoacetamide (compound 14).

後処理

  1. customThe reaction mixture was quenched with H2O
  2. filtrationfiltered
  3. washThe residue was washed with H2O
  4. filtrationfiltered
  5. customrecrystallized from ACN (200 ml)
  6. filtrationThe precipitate was filtered off
  7. customdried

出典と根拠

ORDレコード
ord-0753b49a9b6f4d88adca9743065e65cd
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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