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Water → Methyl 3-[N-(2'-cyanobiphenyl-4-yl)methyl-N-valerylamino]-4-nitrobenzoate

HRID 1655460
ノート
印刷プレビュー

反応式

HRID 1655460 の反応式
[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][C:5]=1[NH:14][C:15](=[O:20])[CH2:16][CH2:17][CH2:18][CH3:19])([O-:3])=[O:2].[C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[C:29]1[CH:36]=[CH:35][C:32]([CH2:33]Br)=[CH:31][CH:30]=1)#[N:22].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[C:29]1[CH:30]=[CH:31][C:32]([CH2:33][N:14]([C:5]2[CH:6]=[C:7]([CH:12]=[CH:13][C:4]=2[N+:1]([O-:3])=[O:2])[C:8]([O:10][CH3:11])=[O:9])[C:15](=[O:20])[CH2:16][CH2:17][CH2:18][CH3:19])=[CH:35][CH:36]=1)#[N:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 15019124'-(Bromomethyl)-2-cyanobiphenylHCID 19792184Methyl 4-nitro-3-valerylaminobenzoate

生成物 1

HCID 19792114Methyl 3-[N-(2'-cyanobiphenyl-4-yl)methyl-N-valerylamino]-4-nitrobenzoate収率 73.8%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of methyl 4-nitro-3-valerylaminobenzoate (1.0 g), 4-(2-cyanophenyl)benzyl bromide (0.97 g) and potassium carbonate (0.55 g) in DMF (10 ml) was stirred for two days at room temperature. To the reaction mixture was added water and the mixture was extracted with ethyl acetate. The organic layer was washed with water and dried. The solvent was distilled off, and the residue was purified by column chromatography on silica gel to afford a pale yellow oil (1.24 g, 73%).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. distillationThe solvent was distilled off
  5. customthe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-116ebd6047f741ec9292c39855af649f
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250554

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート