Hydrochloric Acid → Boc-Leu-Pro-OH

HRID 435395ノート

反応式

HRID 435395 の反応式
[NH:1]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[C@H:2]([C:7]([N:9]1[CH2:23][CH2:22][CH2:21][C@H:10]1[C:11]([O:13]CC1C=CC=CC=1)=[O:12])=[O:8])[CH2:3][CH:4]([CH3:6])[CH3:5].[OH-].[Na+].Cl>CO>[NH:1]([C:24]([O:26][C:27]([CH3:29])([CH3:28])[CH3:30])=[O:25])[C@H:2]([C:7]([N:9]1[CH2:23][CH2:22][CH2:21][C@H:10]1[C:11]([OH:13])=[O:12])=[O:8])[CH2:3][CH:4]([CH3:6])[CH3:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10093486Boc-Leu-Pro-OBn

生成物 1

HCID 1798003Boc-Leu-Pro-OH収率 90.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

BOC-Leu-Pro-OBzl (82.76 g, 0.252 mM) was dissolved in methanol (600 ml). 1 N NaOH (327.6 ml, 1.3 molar excess) was added dropwise with ice cooling, and the mixture was stirred for one hour at room temperature. 1 N HCl (6 ml) was added to the reaction mixture with ice cooling, then the methanol was distilled off in vacuo. After washing the water layer with benzene and ethyl acetate, 1 N HCl (260 ml) was added with ice cooling to form an oily material which was extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution and water and dried with anhydrous sodium sulfate. The solution was dried in vacuo and the residue was dissolved in benzene and lyophilized to obtain the substance [11] (58.57 g, yield: 70.8%).

後処理

  1. distillationthe methanol was distilled off in vacuo
  2. washAfter washing the water layer with benzene and ethyl acetate, 1 N HCl (260 ml)
  3. additionwas added with ice cooling
  4. customto form an oily material which
  5. extractionwas extracted with ethyl acetate
  6. washThe extract was washed with saturated sodium chloride solution and water
  7. dry with materialdried with anhydrous sodium sulfate
  8. customThe solution was dried in vacuo
  9. dissolutionthe residue was dissolved in benzene

出典と根拠

ORDレコード
ord-8daa8b039fd14b8e819f3d8540613691
出典データセット
uspto-grants-1983_08
特許番号
US04400316

反応ノート

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