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

HRID 1296216

反応式

HRID 1296216 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 for 3 hours at room temperature, the solvent was evaporated. The residue was dissolved in ethyl acetate, and successively washed with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was washed with mixture solution of methyl t-butylmethyl ether and hexane, to give 6.97 g of t-butyl N-(5-bromo-2-methoxybenzyl)carbamate.

後処理

  1. customthe solvent was evaporated
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washsuccessively washed 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 mixture solution of methyl t-butylmethyl ether and hexane

出典と根拠

ORDレコード
ord-52512523871d4e4d8e460cff3db66c96
出典データセット
uspto-grants-2007_07
特許番号
US07244861B2

関連ノート

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