N-BOC-ethylenediamine → n-Boc-2-aminoethylguanidine hydroiodide

HRID 566866

反応式

HRID 566866 の反応式
[C:1]([NH:8][CH2:9][CH2:10][NH2:11])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[IH:12].CS[C:15](=[NH:17])[NH2:16]>C(O)C>[IH:12].[C:1]([N:8]([CH2:9][CH2:10][NH2:11])[C:15]([NH2:17])=[NH:16])([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]

参加物

4

反応物 2

HCID 187201N-BOC-ethylenediamineHCID 197812S-methylthiouronium iodide

生成物 1

HCID 23513565n-Boc-2-aminoethylguanidine hydroiodide収率 72.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of commercial N-BOC-ethylendiamine (1 g) in dry ethanol (100 ml) and 2-methyl-2-thiopseudourea hydroiodide (1.5 g) was refluxed for 8 hours. The solvent was removed at reduced pressure and the crude residue purified by flash chromatography (methylene chloride/methanol: 9/1) to yield 1.5 g of N-BOC-2-aminoethylguanidine hydroiodide as a yellow oil which was dissolved in methanolic hydrochloric acid solution 5N (20 ml) and stirred at room temperature for 3 hours. The white precipitate was collected, washed with dry ethanol, affording 700 mg of the intermediate.

後処理

  1. customThe solvent was removed at reduced pressure
  2. customthe crude residue purified by flash chromatography (methylene chloride/methanol: 9/1)

出典と根拠

ORDレコード
ord-5e8fdbaf74cb42bbb3395e3e14e0ff94
出典データセット
uspto-grants-2001_01
特許番号
US06177408B1

関連ノート

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