Hydrochloric Acid → BOC-VAL-GLY-OH

HRID 256493ノート

反応式

HRID 256493 の反応式
[NH:1]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C@H:2]([C:6]([NH:8][CH2:9][C:10]([O:12]CC)=[O:11])=[O:7])[CH:3]([CH3:5])[CH3:4].[OH-].[Na+].Cl>CO>[NH:1]([C:15]([O:17][C:18]([CH3:20])([CH3:19])[CH3:21])=[O:16])[C@H:2]([C:6]([NH:8][CH2:9][C:10]([OH:12])=[O:11])=[O:7])[CH:3]([CH3:4])[CH3:5]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12807303HCID 12807303、化合物

生成物 1

HCID 7014901BOC-VAL-GLY-OH収率 90.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 5.80 g of BOC-Val-Gly-OEt dissolved in 10 ml of methanol, under cooling, was added 23 ml of 1N aqueous sodium hydroxide and the mixture was stirred for one hour, followed by adjustment of pH to 8.0 with 1N hydrochloric acid. The reaction mixture was concentrated under reduced pressure to evaporate methanol, and the aqueous layer was washed with diethyl ether and then adjusted to pH 2.0 with 1N hydrochloric acid. The aqueous layer was extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate, followed by concentration under reduced pressure. The residue was treated with n-hexane and recrystallized from ethyl acetate-n-hexane to give 4.76 g (yield: 90.5%) of BOC-Val-Gly-OH melting at 101° to 107° C. Rf1 =0.20.

後処理

  1. temperatureunder cooling
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customto evaporate methanol
  4. washthe aqueous layer was washed with diethyl ether
  5. extractionThe aqueous layer was extracted with ethyl acetate
  6. dry with materialthe extract was dried over anhydrous sodium sulfate
  7. concentrationfollowed by concentration under reduced pressure
  8. additionThe residue was treated with n-hexane
  9. customrecrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-5f88358dd3a34a78af180e14778f74ce
出典データセット
uspto-grants-1987_10
特許番号
US04703106

反応ノート

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