Water → methyl N-methoxy-N-(3-bromobenzyl)carbamate

HRID 1168038ノート

反応式

HRID 1168038 の反応式
[CH3:1][O:2][NH:3][C:4](=[O:7])[O:5][CH3:6].[H-].[Na+].[Br:10][C:11]1[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=1)[CH2:14]Br.O>CN(C)C=O>[CH3:1][O:2][N:3]([CH2:14][C:13]1[CH:16]=[CH:17][CH:18]=[C:11]([Br:10])[CH:12]=1)[C:4](=[O:7])[O:5][CH3:6]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 699793-Bromobenzyl bromideHCID 12663380methyl N-methoxycarbamate

生成物 1

HCID 22995020methyl N-methoxy-N-(3-bromobenzyl)carbamate収率 455%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.52 g of methyl N-methoxycarbamate in N,N-dimethylformamide (30 ml) was stirred together with 1.15 g of 60% sodium hydride at room temperature for 30 minutes. 1.00 g of 3-bromobenzyl bromide was added dropwise at room temperature, and the resulting solution was stirred for 3 hours. After the reaction, the reaction solution was poured into water and extracted with ethyl acetate, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated under reduced pressure for removal of the solvent. The residue was purified by silica gel column chromatography to give 4.99 g of methyl N-methoxy-N-(3-bromobenzyl)carbamate as a transparent viscous liquid.

後処理

  1. customAfter the reaction
  2. extractionextracted with ethyl acetate
  3. customthe organic layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated under reduced pressure for removal of the solvent
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-243c3e24acc04d54b844e97624f5b8dc
出典データセット
uspto-grants-2003_09
特許番号
US06620961B1

反応ノート

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