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HCID 178516177、化合物 → HCID 178516178、化合物

HRID 268457
ノート
印刷プレビュー

反応式

HRID 268457 の反応式
C([O:8][C:9](=[O:40])[C@H:10]([CH2:30][C:31]1[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=2)[NH:33][CH:32]=1)[NH:11][C:12](=[O:29])[C@H:13]([CH2:23][C:24]1[N:28]=[CH:27][NH:26][CH:25]=1)[NH:14][C:15](=[O:22])[C@@H:16]1[CH2:20][CH2:19][C:18](=[O:21])[NH:17]1)C1C=CC=CC=1>[Pd].C(O)(=O)C>[O:21]=[C:18]1[NH:17][C@H:16]([C:15]([NH:14][C@H:13]([C:12]([NH:11][C@H:10]([C:9]([OH:40])=[O:8])[CH2:30][C:31]2[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[NH:33][CH:32]=2)=[O:29])[CH2:23][C:24]2[N:28]=[CH:27][NH:26][CH:25]=2)=[O:22])[CH2:20][CH2:19]1
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 1

HCID 178516177HCID 178516177、化合物

生成物 1

HCID 178516178HCID 178516178、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

A mixture of N-[N-(5-oxo-L-prolyl)-L-histidyl]-L-tryptophan benzyl ester (Ex. 1, 0.300 g, 0.555 mmol) and 5 percent palladium on carbon (0.060 g) in glacial acetic acid (30 ml) is stirred rapidly under an atmosphere of hydrogen for 16 hours at room temperature. The mixture is filtered through diatomaceous earth ("Celite") and the filtrate is concentrated under reduced pressure. The residue is dissolved in methanol (10 ml) and diethyl ether (100 ml) is slowly added with vigorous stirring. The precipitate is collected, dissolved in methanol (10 ml) and diethyl ether (100 ml) is slowly added. The precipitate is collected, dissolved in methanol, treated with charcoal (0.20 g) and filtered through diatomaceous earth ("Celite"). The filtrate is evaporated to yield the title compound as a hard white glass which is used as such in a subsequent step.

後処理

  1. filtrationThe mixture is filtered through diatomaceous earth ("Celite")
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. dissolutionThe residue is dissolved in methanol (10 ml)
  4. additiondiethyl ether (100 ml) is slowly added with vigorous stirring
  5. customThe precipitate is collected
  6. dissolutiondissolved in methanol (10 ml)
  7. additiondiethyl ether (100 ml) is slowly added
  8. customThe precipitate is collected
  9. dissolutiondissolved in methanol
  10. additiontreated with charcoal (0.20 g)
  11. filtrationfiltered through diatomaceous earth ("Celite")
  12. customThe filtrate is evaporated

出典と根拠

ORDレコード
ord-888d7e7934a241ac8175838b58dc9877
出典データセット
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03947569

反応ノート

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