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

HRID 648269노트

반응식

HRID 648269 반응식
[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]

참가 물질

5

반응물 3

HCID 241Benzene2회HCID 31398Chlorosuccinimide2회HCID 15383894N-(2,6-dimethylphenyl)valine

생성물 1

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

시약·촉매·용매 1

HCID 8058Hexane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d39b5acdf9a14da09347d88c88086c21
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04411912

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