2,4-Dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazine → Methyl 4-((4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-yl)amino)-2-(3-chloropropoxy)benzoate

HRID 400361ノート

反応式

HRID 400361 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[C:4]([O:9][CH2:10][C:11]([F:14])([F:13])[F:12])[N:3]=1.[NH2:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[C:18]([O:26][CH2:27][CH2:28][CH2:29][Cl:30])[CH:17]=1>C1COCC1.C(Cl)Cl.O>[Cl:8][C:6]1[N:5]=[C:4]([O:9][CH2:10][C:11]([F:14])([F:13])[F:12])[N:3]=[C:2]([NH:15][C:16]2[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[C:18]([O:26][CH2:27][CH2:28][CH2:29][Cl:30])[CH:17]=2)[N:7]=1

参加物

6

反応物 2

HCID 580396362,4-Dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazineHCID 67284899Methyl 4-amino-2-(3-chloropropoxy)benzoate

生成物 1

HCID 86664102Methyl 4-((4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-yl)amino)-2-(3-chloropropoxy)benzoate

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2,4-dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazine (770 mg, 2.79 mmol) in THF (10 mL) was added methyl 4-amino-2-(3-chloropropoxy)benzoate (681 mg, 2.79 mmol) and Hunig'sBase (1.464 mL, 8.38 mmol). The resulting mixture was stirred for 16 h. The reaction was diluted with DCM and water. The organic layer was collected and dried over sodium sulfate, and concentrated under vacuum. The crude product was purified by silica gel chromatography using 20-40% EtOAc/Hexanes. The product fractions were collected and concentrated under vacuum to give methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)-2-(3-chloropropoxy)benzoate as a solid.

後処理

  1. customThe organic layer was collected
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under vacuum
  4. customThe crude product was purified by silica gel chromatography
  5. customThe product fractions were collected
  6. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-58ee575fb1c44abf9b534308bd2b810c
出典データセット
uspto-grants-2014_06
特許番号
US08741884B2

反応ノート

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