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Sodium Hydroxide → Boc-D-Met-Gly-OH

HRID 1277396
ノート
印刷プレビュー

反応式

HRID 1277396 の反応式
[NH:1]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[C@@H:2]([C:7]([NH:9][CH2:10][C:11]([O:13]CC)=[O:12])=[O:8])[CH2:3][CH2:4][S:5][CH3:6].[OH-].[Na+]>C(O)C>[NH:1]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[C@@H:2]([C:7]([NH:9][CH2:10][C:11]([OH:13])=[O:12])=[O:8])[CH2:3][CH2:4][S:5][CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 12919642Ethyl (tert-butoxycarbonyl)-D-methionylglycinate

生成物 1

HCID 7019049Boc-D-Met-Gly-OH収率 88.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 20 ml of ethyl alcohol is dissolved 4.7 g of BOC-(D)-Met-Gly-OEt. After cooling, 16 ml of N-aqueous sodium hydroxide solution is added, and the mixture is stirred at room temperature for 1 hour. The ethyl alcohol is distilled off, and the residue, after adding aqueous citric acid solution to neutralize, is extracted with 100 ml of ethyl acetate, followed by washing with water and drying over anhydrous sodium sulphate. The AcOEt isdistilled off and the residue is crystallized with petroleum ether. Recrystallization from AcOEt-petroleum ether results in a yield of 3.8 g of the desired product, m.p. 124°-125° C., Rf1 =0.41, [α]D21 +12.3° (c=0.59, DMF)

後処理

  1. temperatureAfter cooling
  2. distillationThe ethyl alcohol is distilled off
  3. additionthe residue, after adding aqueous citric acid solution
  4. extractionis extracted with 100 ml of ethyl acetate
  5. washby washing with water
  6. dry with materialdrying over anhydrous sodium sulphate
  7. customthe residue is crystallized with petroleum ether
  8. customRecrystallization from AcOEt-petroleum ether

出典と根拠

ORDレコード
ord-a77c89b20aa945c790e5a050c1296726
出典データセット
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04277394

反応ノート

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