Water → HCID 86691693、化合物

HRID 522266

反応式

HRID 522266 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 86691693HCID 86691693、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-eafeb1729d4047ca972518043fa6f237
出典データセット
uspto-grants-2016_05
特許番号
US09328118B2

関連ノート

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