Water → HCID 86691693, 화합물

HRID 522266

반응식

HRID 522266 반응식
CN.[CH2:3]([N:5](CC)CC)C.[Cl:10][C:11]1[N:16]=[C:15]([Cl:17])[C:14]([N+:18]([O-:20])=[O:19])=[C:13](Cl)[N:12]=1.O>C1COCC1.CCOC(C)=O>[Cl:10][C:11]1[N:12]=[C:13]([NH:5][CH3:3])[C:14]([N+:18]([O-:20])=[O:19])=[C:15]([Cl:17])[N:16]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 6329MethylamineHCID 8471TriethylamineHCID 42978432,4,6-Trichloro-5-nitropyrimidine

생성물 1

HCID 86691693HCID 86691693, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

A 2 M solution of methylamine and triethylamine (1.8 mL) in THF (4.6 mL) were added to a solution of 2,4,6-trichloro-5-nitropyrimidine (2 g) in THF (30 mL) under ice-cooling, and the mixture was stirred for 1 hour under ice-cooling. After water was added to the reaction mixture, extraction thereof was performed using EtOAc, and the extract was washed with water and saturated brine. The organic layer was dried over MgSO4 and filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (Hex:EtOAc=99:1 to 90:10), whereby 2,6-dichloro-N-methyl-5-nitropyrimidine-4-amine (680 mg) was obtained as a pale yellow solid.

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. washthe extract was washed with water and saturated brine
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (Hex:EtOAc=99:1 to 90:10)

출처 및 근거

ORD 기록
ord-eafeb1729d4047ca972518043fa6f237
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328118B2

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