Triethylamine → 5-[4-(4-Methoxy-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine

HRID 2294038

반응식

HRID 2294038 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:5][CH:4]=1.C(N(CC)CC)C.Br.Br.Br[CH2:25][C:26]1[C:27]([NH2:33])=[N:28][C:29]([NH2:32])=[N:30][CH:31]=1>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([CH2:25][C:26]3[C:27]([NH2:33])=[N:28][C:29]([NH2:32])=[N:30][CH:31]=3)[CH2:11][CH2:10]2)=[CH:7][CH:8]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2697221-(4-Methoxyphenyl)piperazineHCID 214736085-(Bromomethyl)pyrimidine-2,4-diamine dihydrobromide

생성물 1

HCID 214736195-[4-(4-Methoxy-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine수율 47%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 0.95 g (0.00494 mol) of 1-(4-methoxy-phenyl)-piperazine in 30 ml of dimethylformamide was treated with 1.37 ml (0.00986 mol) of triethylamine and 0.60 g (0.00164 mol) of 5-bromomethyl-pyrimidine-2,4-diamine dihydrobromide and the mixture was stirred at room temperature under argon for 65 hours. The mixture was completely freed from the solvents. The residue was chromatographed over silica gel with acetonitrile/methanol (1:1 ), digested in diethyl ether and subsequently filtered off under suction. 0.24 g (47%) of 5-[4-(4-methoxy-phenyl)-piperazin-1-ylmethyl]-pyrimidine-2,4-diamine was obtained as white crystals; m.p. 239°-241°.

후처리

  1. customThe residue was chromatographed over silica gel with acetonitrile/methanol (1:1 )
  2. filtrationsubsequently filtered off under suction

출처 및 근거

ORD 기록
ord-c97c882a7aa249c09f11774b320d1579
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05688798

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