Hydrochloric Acid → HCID 131711700、化合物

HRID 2052273ノート

反応式

HRID 2052273 の反応式
[NH:1](C(OC(C)(C)C)=O)[C@H:2]([C:13]([NH:15][C@H:16]([C:21]([NH:23][C@H:24]([C:29]([NH:31][C@@H:32]([C:39]([NH2:41])=[O:40])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=[O:30])[CH2:25][C:26](=[O:28])[OH:27])=[O:22])[CH2:17][CH2:18][CH2:19][CH3:20])=[O:14])[CH2:3][C:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1.[ClH:49].SC(O)C>O1CCOCC1>[NH2:1][C@H:2]([C:13]([NH:15][C@H:16]([C:21]([NH:23][C@H:24]([C:29]([NH:31][C@@H:32]([C:39]([NH2:41])=[O:40])[C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=[O:30])[CH2:25][C:26](=[O:27])[OH:28])=[O:22])[CH2:17][CH2:18][CH2:19][CH3:20])=[O:14])[CH2:3][C:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1.[ClH:49]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4713212Mercapto-ethanolHCID 131711697HCID 131711697、化合物

生成物 1

HCID 131711700HCID 131711700、化合物収率 99%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2.20 g (3.32 mmoles) of BOC-Trp-Nle-Asp-D-Phg-NH2 are treated with 25 ml of 4 n hydrochloric acid in dioxane in the presence of 1.20 ml (17 mmoles) of mercaptoethanol. After 15 minutes the solution is evaporated in vacuo, the residue is triturated with ether, and the solid is filtered off. 1.99 g (99.0%) of H-Trp-Nle-Asp-D-Phg-NH2.HCl are obtained; m.p.: 217°-221° C. (decomposition), Rf7 :0.35, [α]D :-54.2° (c: 1.0, in dimethyl formamide).

後処理

  1. customAfter 15 minutes the solution is evaporated in vacuo
  2. customthe residue is triturated with ether
  3. filtrationthe solid is filtered off

出典と根拠

ORDレコード
ord-ee3ef9bcea594fca964243d3187c2396
出典データセット
uspto-grants-1980_01
特許番号
US04183909

反応ノート

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