Dichloromethane → 6-Methyl-5-[4-(2-furoyl)piperazin-1-ylmethyl]-4-(3-nitrophenyl)-2-phenylpyrimidine

HRID 4689

反応式

HRID 4689 の反応式
Cl.Cl.[CH3:3][C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[C:6]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-:24])=[O:23])[CH:17]=2)[C:5]=1[CH2:25][N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.ClCCl.[O:35]1[CH:39]=[CH:38][CH:37]=[C:36]1[C:40](Cl)=[O:41]>C(N(CC)CC)C>[CH3:3][C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[C:6]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-:24])=[O:23])[CH:17]=2)[C:5]=1[CH2:25][N:26]1[CH2:31][CH2:30][N:29]([C:40]([C:36]2[O:35][CH:39]=[CH:38][CH:37]=2)=[O:41])[CH2:28][CH2:27]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 682422-Furancarbonyl chlorideHCID 201513906-Methyl-5-(1-piperazinylmethyl)-4-(3-nitrophenyl)-2-phenylpyrimidine dihydrochloride

生成物 1

HCID 201514026-Methyl-5-[4-(2-furoyl)piperazin-1-ylmethyl]-4-(3-nitrophenyl)-2-phenylpyrimidine収率 97.5%

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To a mixture of 6-methyl-5-(1-piperazinylmethyl)-4-(3-nitrophenyl)-2-phenylpyrimidine dihydrochloride (1 g), dichloromethane (10 ml) and triethylamine (0.48 g), was added 2-furoyl chloride (0.31 g) at 5° C. under ice cooling. After stirring for 1 hour at the same temperature, the reaction mixture was concentrated under reduced pressure. The residue was suspended in water and adjusted to pH=9 with aqueous saturated sodium hydrogen carbonate. The precipitate was collected by filtration, washed with water and dried in vacuo to give 6-methyl-5-[4-(2-furoyl)piperazin-1-ylmethyl]-4-(3-nitrophenyl)-2-phenylpyrimidine (1.02 g).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-1b0e899e852c46f697084b105512427c
出典データセット
uspto-grants-1988_02
特許番号
US04727073

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