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

HRID 566866

반응식

HRID 566866 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 23513565n-Boc-2-aminoethylguanidine hydroiodide수율 72.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-5e8fdbaf74cb42bbb3395e3e14e0ff94
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06177408B1

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