Dichloromethane → 4,5-Dimethyl-2-(4-methylphenyl)pyrimidine

HRID 1077836노트

반응식

HRID 1077836 반응식
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6](Cl)[N:5]=[C:4]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)[N:3]=1.C(N(CC)CC)C.C(Cl)Cl>[Pd].CO>[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([C:10]2[CH:15]=[CH:14][C:13]([CH3:16])=[CH:12][CH:11]=2)[N:3]=1

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 194302834,5-Dimethyl-6-chloro-2-(4-methylphenyl)pyrimidine

생성물 1

HCID 194302024,5-Dimethyl-2-(4-methylphenyl)pyrimidine수율 83.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of 4,5-dimethyl-6-chloro-2-(4-methylphenyl)pyrimidine (6.2 g), triethylamine (3.2), and palladium on carbon (200 mg) in 100 ml of methanol was stirred overnight under hydrogen. Methylene chloride was added, the solid filtered off through celite, and solvent removed from the filtrate under reduced pressure. Tetrahydrofuran was added to the residue, and triethylamine hydrochloride filtered off. Solvent was removed from the filtrate under reduced pressure, giving 4.4 g of 4,5-dimethyl-2-(4-methylphenyl)pyrimidine, m.p. 114° C.

후처리

  1. filtrationthe solid filtered off through celite, and solvent
  2. customremoved from the filtrate under reduced pressure
  3. additionTetrahydrofuran was added to the residue, and triethylamine hydrochloride
  4. filtrationfiltered off
  5. customSolvent was removed from the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-b32b856a98264bdb8efc8602e4b085d5
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05545645

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