Ethyl Acetate → 1-Methyl-4-[[3-nitro-5-(trifluoromethyl)phenyl]methyl]piperazine

HRID 2200147ノート

反応式

HRID 2200147 の反応式
Cl[CH2:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[C:5]([N+:13]([O-:15])=[O:14])[CH:4]=1.[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.CCOC(C)=O>C1COCC1>[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:2][C:3]2[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:6]=[C:5]([N+:13]([O-:15])=[O:14])[CH:4]=2)[CH2:19][CH2:18]1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 531671-MethylpiperazineHCID 684250951-(Chloromethyl)-3-nitro-5-(trifluoromethyl)benzene

生成物 1

HCID 589023661-Methyl-4-[[3-nitro-5-(trifluoromethyl)phenyl]methyl]piperazine収率 100%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Stir the mixture of 1-(chloromethyl)-3-nitro-5-(trifluoromethyl)benzene (640 mg, 2.68 mmol) and N-methylpiperazine (536 mg, 5.36 mmol) in THF (8 mL) for 2 hrs at 60° C. TLC (EtOAc:PE=1:1) shows the reaction is complete. Concentrate the reaction mixture under reduced pressure to obtain the crude product (812 mg, 100%). MS: (M+1): 303.1.

後処理

  1. concentrationConcentrate the reaction mixture under reduced pressure

出典と根拠

ORDレコード
ord-910e5f43cdc44a3db6714126dc657e98
出典データセット
uspto-grants-2016_06
特許番号
US09359338B2

反応ノート

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