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Hydrogen Peroxide → BOC-Tyr-(D)-Met(O)-Gly-OH

HRID 1277395
ノート
印刷プレビュー

反応式

HRID 1277395 の反応式
[NH:1]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[C@H:2]([C:11]([NH:13][C@@H:14]([C:19]([NH:21][CH2:22][C:23]([OH:25])=[O:24])=[O:20])[CH2:15][CH2:16][S:17][CH3:18])=[O:12])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1.OO.CN(C=[O:39])C>CO.C(O)(=O)C.[Pd]>[NH:1]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[C@H:2]([C:11]([NH:13][C@@H:14]([C:19]([NH:21][CH2:22][C:23]([OH:25])=[O:24])=[O:20])[CH2:15][CH2:16][S:17]([CH3:18])=[O:39])=[O:12])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 784Hydrogen PeroxideHCID 6228DimethylformamideHCID 12919645N-(tert-Butoxycarbonyl)-L-tyrosyl-D-methionylglycine

生成物 1

HCID 12919648BOC-Tyr-(D)-Met(O)-Gly-OH

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒
HCID 887
Methanol
溶媒

実験手順

In a mixed solvent comprising 10 ml of MeOH and 5 ml of acetic acid is dissolved 2.2 g of BOC-Tyr-(D)-Met-Gly-OH, followed by adding 0.6 ml of 30% aqueous hydrogen peroxide solution, and the mixture is stirred at roomtemperature for 5 hours. Following the addition of a small amount of palladium black, the mixture is stirred. The catalyst is filtered out, andthe solvent is distilled off, whereby the precipitated crystals are collected by filtration. Thus obtained is 2.1 g of the desired product, m.p. 185° C. (decomposed), Rf1 =0.20, [α]D21 +1.8° (c=0.5, DMF)

後処理

  1. stirringthe mixture is stirred
  2. filtrationThe catalyst is filtered out
  3. distillationandthe solvent is distilled off
  4. filtrationwhereby the precipitated crystals are collected by filtration
  5. customThus obtained

出典と根拠

ORDレコード
ord-18cf99727005470b972861d354daf2ae
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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