1,3-Dithiolane → Diethylether ethylacetate

HRID 439398

反応式

HRID 439398 の反応式
S1CCSC1.C(C(N[C@H](C(N[C@H:30]([C:38]([O:40][CH2:41][CH3:42])=[O:39])CC1C=CC=CC=1)=O)CC(C)C)=O)(C1C=CC=CC=1)C1C=CC=CC=1.NCCCN1[CH2:52][CH2:51][O:50][CH2:49][CH2:48]1>>[CH3:42][CH2:41][O:40][C:38]([CH3:30])=[O:39].[CH3:48][CH2:49][O:50][CH2:51][CH3:52]

参加物

4

反応物 3

HCID 209701,3-DithiolaneHCID 61055N-(3-Aminopropyl)morpholineHCID 131719396Ph2CHCO-Leu-Phe-COOEt

生成物 1

HCID 21584169Diethylether ethylacetate収率 20%

実験手順

This compound was synthesized from 1,3-dithiolane derivative of Ph2CHCO-Leu-Phe-COOEt and N-aminopropylmorpholine, and purified by column chromatography using AcOEt followed by crystallization from AcOEt/ether (20% yield). Yellow solid, single spot on TLC, Rf =0.45 (AcOET/CH3OH 9:1), mp 158°-160° C. 1H NMR (CDCl3) ok, MS (FAB) m/e=627 (M+1). Anal: calcd. for C37H46N4O5, 626; C, 70.90; H, 7.40; N, 8.94. Found, C, 70.05; H, 7.43; N, 8.68.

後処理

  1. custompurified by column chromatography

出典と根拠

ORDレコード
ord-a0c4a16670544afa9b01d20d786d28fa
出典データセット
uspto-grants-1996_05
特許番号
US05514694

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