Triethylamine → 4,6-Dichloro-2-(3-isopropoxypropylamino)-5-methylthiopyrimidine

HRID 65381ノート

反応式

HRID 65381 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[C:5]([S:9][CH3:10])=[C:4]([Cl:11])[N:3]=1.C(N(CC)CC)C.[CH:19]([O:22][CH2:23][CH2:24][CH2:25][NH2:26])([CH3:21])[CH3:20]>C1(C)C=CC=CC=1>[Cl:11][C:4]1[C:5]([S:9][CH3:10])=[C:6]([Cl:8])[N:7]=[C:2]([NH:26][CH2:25][CH2:24][CH2:23][O:22][CH:19]([CH3:21])[CH3:20])[N:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 761943-IsopropoxypropylamineHCID 122255442,4,6-Trichloro-5-methylsulfanyl-pyrimidine

生成物 1

HCID 135798934,6-Dichloro-2-(3-isopropoxypropylamino)-5-methylthiopyrimidine収率 27.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

68.5 g (0.3 mole) of 2,4,6-trichloro-5-methylthiopyrimidine are dissolved in 300 ml of toluene. 30.3 g (0.3 mole) of triethylamine and 35.1 g (0.3 mole) of isopropoxypropylamine are added dropwise at 0° C. After the mixture had been subsequently stirred at room temperature for 1 hour, it is diluted with 500 ml of toluene and the organic phase is washed with water. After drying over sodium sulphate and removal of the solvent in vacuo, the resulting residue is stirred with 100 ml of petroleum ether, filtered off with suction, rinsed with petroleum ether and dried. 25.3 g (27.2% of theory) of the above-mentioned pyrimidine, melting point: 88° C., are thus obtained.

後処理

  1. washthe organic phase is washed with water
  2. dry with materialAfter drying over sodium sulphate and removal of the solvent in vacuo
  3. stirringthe resulting residue is stirred with 100 ml of petroleum ether
  4. filtrationfiltered off with suction
  5. washrinsed with petroleum ether
  6. customdried

出典と根拠

ORDレコード
ord-8da94d8fab044e368db50f6bb8487cc1
出典データセット
uspto-grants-1986_09
特許番号
US04614532

反応ノート

読み込み中…