Benzene → N-(2,6-dimethyl-4-chlorophenyl)valine

HRID 1389364ノート

反応式

HRID 1389364 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C@H:10]([C:14]([OH:16])=[O:15])[CH:11]([CH3:13])[CH3:12].[Cl:17]N1C(=O)CCC1=O.C1C=CC=CC=1>CCCCCC>[CH3:8][C:4]1[CH:5]=[C:6]([Cl:17])[CH:7]=[C:2]([CH3:1])[C:3]=1[NH:9][C@H:10]([C:14]([OH:16])=[O:15])[CH:11]([CH3:12])[CH3:13]

参加物

5

反応物 3

HCID 241Benzene2 回HCID 31398Chlorosuccinimide2 回HCID 15383894N-(2,6-dimethylphenyl)valine

生成物 1

HCID 54357344N-(2,6-dimethyl-4-chlorophenyl)valine

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒2 回

実験手順

A mixture of 0.5 g of the m-phenoxybenzyl ester of N-(2,6-dimethylphenyl)valine, 0.21 g of N-chlorosuccinimide and 3 ml of benzene is heated at reflux for 2 hours. The reaction is diluted with hexane, washed with water (2×) and solvent stripped to give the crude product. To the crude product is added 0.1 g of N-chlorosuccinimide and 3 ml benzene. The mixture is heated at reflux for 30 min and then allowed to stand overnight at RT. The reaction is worked up by diluting with hexane, washing with water and stripping off solvent to yield the m-phenoxybenzyl ester of N-(2,6-dimethyl-4-chlorophenyl)valine, MS m/e 437.1 (M+, 15.3).

後処理

  1. temperatureis heated
  2. temperatureat reflux for 2 hours
  3. washwashed with water (2×) and solvent
  4. customto give the crude product
  5. temperatureThe mixture is heated
  6. temperatureat reflux for 30 min
  7. washwashing with water

出典と根拠

ORDレコード
ord-19aa7d2976cb474ca6a7d9bd85459df1
出典データセット
uspto-grants-1981_01
特許番号
US04243819

反応ノート

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