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 400361노트

반응식

HRID 400361 반응식
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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-58ee575fb1c44abf9b534308bd2b810c
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741884B2

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