Ethylamine → HCID 7038767、化合物

HRID 247514ノート

反応式

HRID 247514 の反応式
[NH:1]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C@@H:2]([C:7]([OH:9])=O)[CH2:3][CH:4]([CH3:6])[CH3:5].O.C[N:19]1CCO[CH2:21][CH2:20]1.C(Cl)(=O)OCC.C(N)C>C1COCC1>[NH:1]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[C@@H:2]([C:7]([NH:19][CH2:20][CH3:21])=[O:9])[CH2:3][CH:4]([CH3:5])[CH3:6]

参加物

6

反応物 4

HCID 6341EthylamineHCID 79724-MethylmorpholineHCID 10928Ethyl chloroformateHCID 2724763D-Leucine, N-[(1,1-dimethylethoxy)carbonyl]-, monohydrate

生成物 1

HCID 7038767HCID 7038767、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-20 °C

実験手順

25 g of Boc-D-Leu-OH.H2O was dissolved in 200 ml of THF. The solution was cooled to -20° C. 11 ml of N-methylmorpholine and 9.56 ml of ethyl chlorocarbonate were added to the solution. After 5 min, 12.9 g of a 70% aqueous ethylamine solution was added thereto and the mixture was stirred at about -5° C. for 2 h. After concentration, the residue was dissolved in ethyl acetate and washed with an aqueous NaHCO3 solution and water successively. After concentration to dryness, 24.5 g of Boc-D-Leu-NHC2H5 was obtained.

後処理

  1. concentrationAfter concentration
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with an aqueous NaHCO3 solution and water successively
  4. concentrationAfter concentration to dryness

出典と根拠

ORDレコード
ord-de080da5d0764931831bd1dba3bd98c8
出典データセット
uspto-grants-1987_11
特許番号
US04707468

反応ノート

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