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

HRID 1077836ノート

反応式

HRID 1077836 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b32b856a98264bdb8efc8602e4b085d5
出典データセット
uspto-grants-1996_08
特許番号
US05545645

反応ノート

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