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

HRID 65381노트

반응식

HRID 65381 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8da94d8fab044e368db50f6bb8487cc1
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614532

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