2,4,5-Trichlorophenol → N-(1,1-dimethylethoxycarbonyl)leucine 2,4,5-trichlorophenyl ester

HRID 53085

反応式

HRID 53085 の反応式
[CH3:1][C:2]([CH3:16])([O:4][C:5]([NH:7][C@H:8]([C:13]([OH:15])=[O:14])[CH2:9][CH:10]([CH3:12])[CH3:11])=[O:6])[CH3:3].[Cl:17][C:18]1[CH:23]=[C:22]([Cl:24])[C:21]([Cl:25])=[CH:20][C:19]=1O.C1(N=C=NC2CCCCC2)CCCCC1>C(OCC)(=O)C>[Cl:17][C:18]1[CH:23]=[C:22]([Cl:24])[C:21]([Cl:25])=[CH:20][C:19]=1[O:14][C:13](=[O:15])[C@H:8]([CH2:9][CH:10]([CH3:12])[CH3:11])[NH:7][C:5]([O:4][C:2]([CH3:3])([CH3:1])[CH3:16])=[O:6]

参加物

5

反応物 3

HCID 72712,4,5-TrichlorophenolHCID 10868DicyclohexylcarbodiimideHCID 83170L-Leucine, N-((1,1-dimethylethoxy)carbonyl)-

生成物 1

HCID 15431614N-(1,1-dimethylethoxycarbonyl)leucine 2,4,5-trichlorophenyl ester収率 100.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

N-(1,1-Dimethylethoxycarbonyl)leucine (6.32 g, 15 mmol) was stirred with 2,4,5-trichlorophenol (3.01 g, 15.2 mmol) and dicyclohexylcarbodiimide (3.14 g, 15.2 mmol) in ethyl acetate (50 mL) at -10° C. for 4 h. The suspension was filtered and the solvent was evaporated under reduced pressure from the filtrate. The residue was dissolved in ethyl acetate. The suspension was filtered and the solvent was evaporated under reduced pressure from the filtrate to give N-(1,1-dimethylethoxycarbonyl)leucine 2,4,5-trichlorophenyl ester (6.2 g, 99%).

後処理

  1. filtrationThe suspension was filtered
  2. customthe solvent was evaporated under reduced pressure from the filtrate
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. filtrationThe suspension was filtered
  5. customthe solvent was evaporated under reduced pressure from the filtrate

出典と根拠

ORDレコード
ord-03579b5b559c4d1b83d5f3479325a6db
出典データセット
uspto-grants-1997_04
特許番号
US05618528

関連ノート

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