N-bromobutanimide → Tert-butyl (5-bromo-2-methoxybenzyl)carbamate

HRID 1985293

反応式

HRID 1985293 の反応式
[CH3:1][O:2][C:3]1[CH:17]=[CH:16][CH:15]=[CH:14][C:4]=1[CH2:5][NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10].[Br:18]N1C(=O)CCC1=O>C(#N)C>[Br:18][C:15]1[CH:16]=[CH:17][C:3]([O:2][CH3:1])=[C:4]([CH:14]=1)[CH2:5][NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:10])[CH3:11]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 22926021Tert-butyl (2-methoxybenzyl)carbamate

生成物 1

HCID 22926030Tert-butyl (5-bromo-2-methoxybenzyl)carbamate収率 86.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

6.04 g of t-Butyl N-(2-methoxybenzyl)carbamate was dissolved in 50 ml of acetonitrile, and 4.6 g of N-bromosuccinimide was added. After stirring was continued at room temperature for 3 hours, the solvent was evaporated. The residue was dissolved in ethyl acetate, and washed successively with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was washed with a mixed solution of methyl t-butyl ether and hexane, to give 6.97 g of the title compound.

後処理

  1. customthe solvent was evaporated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed successively with water and saturated brine
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated
  6. washThe residue was washed with a mixed solution of methyl t-butyl ether and hexane

出典と根拠

ORDレコード
ord-7df243ff2a4f4008a919224b26af209b
出典データセット
uspto-grants-2009_06
特許番号
US07544835B2

関連ノート

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